2,6-DIFORMYLPHENOL

Weigh 940.5 mg of phenol and 2.80 g of hexamethylenetetramine into a 100 mL glass reaction bottle with a balance and add30mL of trifluoroacetic acid, put into a clean small magnet, and then use the 84-1 magnetic stirring temperature control electric heating sleeve to heat the reflux.Record the reaction time, use the thin-layer chromatography silica gel plate to track the progress of the reaction, about 6h reaction, after the reaction is complete, turn offreaction. For the synthesis reaction, see Formula I:Formula I: Synthesis of 2, 6-DiformylphenolPrepare a 100 mL beaker and pour about 50 mL of distilled water into it. After the reaction stops, after cooling, it will be reversed.The solution should be added dropwise to the beaker prepared in advance.Stir well with a dropper, pour the liquid in the beaker into the separatory funnel, and add about 20 mL to it.Methylene chloride, tighten the plug and shake it a few times, then place the separatory funnel on the iron frame and let it stand for a few minutes to make the liquidFloor. Since the density of methylene chloride is larger than that of water, the dichloromethane solution is below, our product is organic, generally notSoluble in water, so that the extraction process is completely soluble in dichloromethane. Open the piston of the separatory funnel and let the dichloromethane flow from the lower partOut. Then, add about 20 mL of dichloromethane to the remaining liquid in the separatory funnel, and repeat 3 to 5 repeatedly.The product is completely distilled into the dichloromethane.After the extraction, weigh a 25mL glass reaction bottle, and use this flask to extract the two we obtained.The methyl chloride liquid was spun dry using a rotary evaporator. Then take a little spin dry material in a 4mL centrifuge tube, then add a small amount of twoMethyl chloride was dissolved, a small amount of solution was removed with a glass capillary, and the plate was plated on a thin layer chromatography silica gel plate, followed by thin layer chromatography.Place the silica gel plate in a glass jar containing about 1 mL of methylene chloride, wait for about 3 minutes, wait until the dichloromethane liquid is going to be thin.When the chromatographic silica gel plate is completely wetted, the thin layer chromatography silica gel plate is taken out with tweezers, and the 365 nm in a portable ultraviolet analyzer is used.When the fluorescent lamp is excited, a fluorescent spot can be observed. When the fluorescent lamp is excited by 254 nm, there is no other point, indicating that the extraction is dry.The solid obtained afterwards is relatively pure and can be directly reacted to the next reaction. After the flask is cooled, weigh it again and the weight of the product is976.5 mg, the yield was 65.1percent.Weigh 940.5 mg of phenol and 2.80 g of hexamethylenetetramine into a 100 mL glass reaction bottle with a balance.Add 30 mL of trifluoroacetic acid, Put in a clean little magnet, Then use 84-1 magnetic stirring temperature control electric heating sleeve to heat the reflux, Record the reaction time, The thin layer chromatography silica gel plate was used to track the progress during the reaction.It takes about 6 hours to react.After the reaction is complete, Turn off the reaction.For the synthesis reaction, see Formula I:Prepare a 100 mL beaker and pour about 50 mL of distilled water into it. After the reaction stops, after cooling, it will be reversed.The solution should be added dropwise to the beaker prepared in advance.Stir well with a dropper, pour the liquid in the beaker into the separatory funnel, and add about 20 mL to it.Methylene chloride, tighten the plug and shake it a few times, then place the separatory funnel on the iron frame and let it stand for a few minutes to make the liquidFloor. Since the density of methylene chloride is larger than that of water, the dichloromethane solution is below, our product is organic, generally notSoluble in water, so that the extraction process is completely soluble in dichloromethane. Open the piston of the separatory funnel and let the dichloromethane flow from the lower partOut. Then, add about 20 mL of dichloromethane to the remaining liquid in the separatory funnel, and repeat 3 to 5 repeatedly.The product is completely distilled into the dichloromethane.After the extraction, weigh a 25mL glass reaction bottle, and use this flask to extract the two we obtained.The methyl chloride liquid was spun dry using a rotary evaporator. Then take a little spin dry material in a 4mL centrifuge tube, then add a small amount of twoMethyl chloride was dissolved, a small amount of solution was removed with a glass capillary, and the plate was plated on a thin layer chromatography silica gel plate, followed by thin layer chromatography.Place the silica gel plate in a glass jar containing about 1 mL of methylene chloride, wait for about 3 minutes, wait until the dichloromethane liquid is going to be thin.When the chromatographic silica gel plate is completely wetted, the thin layer chromatography silica gel plate is taken out with tweezers, and the 365 nm in a portable ultraviolet analyzer is used.When the fluorescent lamp is excited, a fluorescent spot can be observed. When the fluorescent lamp is excited by 254 nm, there is no other point, indicating that the extraction is dry.The solid obtained afterwards is relatively pure and can be directly reacted to the next reaction. After the flask is cooled, weigh it again and the weight of the product is976.5 mg, the yield was 65.1percent.The balance for weighing the phenol 940.5 mg and hexamethylene tetramine 2.80 g is put into a 100 ml glass bottle in the reaction, by adding 30 ml of trifluoroacetic acid, placed into a washing clean small magneton, followed by a 84 - 1 magnetic stirring and temperature control jacket with heating to reflux, recording the reaction time, the reaction process by using thin layer chromatography silica gel plate in the tracking process, about reaction 6 h, after the reaction is complete, turn off the reaction. Synthesizing the response sees the type I:Type I: 2, 6 - dimethyl phenol synthesis of acylTo a 100 ml beaker, in wherein the tipped into the 50 ml of distilled water to the left and the right. In the reaction stops, after cooling, the reaction solution is prepared in advance in [...] in the beaker, A dropper and stir, the beaker in the liquid is poured in to the separatory funnel, then wherein add 20 ml dichloromethane left, several fastening plug firmly under shaking, after the separatory funnel will be placed on the iron stand standing a few minutes, the liquid layer. The dichloromethane density than water is large, so the dichloromethane solution below, our product is organic matter, generally not soluble in water, thus extracting process completely dissolved in dichloromethane. The piston of the separatory funnel, the methylene chloride from the lower outflow. Then remaining in the separatory funnel in the liquid by adding 20 ml of dichloromethane extraction left, so repeated repeated 3 to 5 times, make the product fully enter into the dichloromethane.In the extraction end after, weighing a 25 ml glass reaction bottle, this flask for our extraction obtained dichloromethane liquid for the Rotavapor turns on lathe does. Then fetch a little turns on lathe does material in 4 ml of in a centrifuge tube, add a small amount of dichloromethane to dissolve, glass capillary solution of a little solution, in thin layer chromatography silica gel plate and the point on the plate, after the thin layer chromatography silica gel plate into the containing about 1 ml methylene chloride in wide-mouth bottle glass, about to wait for 3 mi n, wait until the dichloromethane liquid will soon be thin layer chromatography silica gel plate when all wetted for the thin layer chromatography silica gel plate taken out of the tweezers, using hand-held ultraviolet analyzer in the 365 nm fluorescent lamp excitation, can be observed a keyswitch, in the 254 nm fluorescent lamp when excited, no other point, turns on lathe does note obtained after extraction of solid relatively pure, can be directly cast one-step reaction. The flask after cooling and again weighing, the weight of the obtained product 976.5 mg, yield is 65.1percent.General procedure: To a solution of substrates (1a–1q, 0.15 mmol) in trifluoroacetic acid (5 ml), hexamethylenetetramine (0.3 mmol) and cuprous oxide (0.15 mmol) were added. The reaction mixture was refluxed for about 5 h, cooled to room temperature, followed by addition of hydrochloric acid (3 N, 5 ml). After stirring for another 1 h, the solution was concentrated under reduced pressure. The products were purified by silica gel column chromatography (200–300 mesh).Weigh phenol 940.5mg and balance with a balanceHexamethylenetetramine2.80g into 100mLGlass reaction bottle, Add 30 mL of trifluoroacetic acid, Put in a clean little magnet, Then use 84-1 magnetic stirring temperature control electric heating sleeve to heat the reflux, Record the reaction time, The thin layer chromatography silica gel plate was used to track the progress during the reaction.It takes about 6 hours to react.After the reaction is complete, Turn off the reaction.For the synthesis reaction, see Formula I:Formula I: Synthesis of 2, 6-DiformylphenolPrepare a 100mL beaker, Pour about 50 mL of distilled water into it.When the reaction stops, After cooling, The reaction solution is added dropwise to a beaker prepared in advance, Stir well with a dropper, Pour the liquid from the beaker into the separatory funnel.Then add about 20 mL of dichloromethane to it.Tighten the plug and shake it a few timesThen, place the separatory funnel on the iron frame and let it stand for a few minutes.Layer the liquid.Since the density of methylene chloride is larger than water, So the dichloromethane solution is below, Our products are organicGenerally not soluble in water, Thus the extraction process is completely soluble in dichloromethane.Open the piston of the separatory funnel, The dichloromethane was allowed to flow out from the lower portion.Then add about 20 mL of dichloromethane to the remaining liquid in the separatory funnel., repeating this 3 to 5 times, Allow the product to completely enter the dichloromethane.After the extraction, Weighing a 25mL glass reaction bottle, Using this flask, the dichloromethane liquid obtained by our extraction was spin-dried using a rotary evaporator.Then take a little spin dry material in a 4mL centrifuge tube, add a small amount of methylene chloride to dissolve it.Use a glass capillary to remove a small amount of solution.Plate on a thin layer chromatography silica gel plate, The thin layer chromatography silica gel plate was then placed in a glass jar containing about 1 mL of methylene chloride, and waited for about 3 minutes until the dichloromethane liquid was soon thin.When the chromatographic silica gel plate is completely wetted, the thin layer chromatography silica gel plate is taken out with tweezers, and the 365 nm in a portable ultraviolet analyzer is used.When the fluorescent lamp is excited, a fluorescent spot can be observed. When the fluorescent lamp is excited by 254 nm, there is no other point, indicating that the extraction is dry.The solid obtained afterwards is relatively pure and can be directly reacted to the next reaction. After the flask is cooled, weigh it again and the weight of the product is976.5 mg, the yield was 65.1percent

Molecular Weight:150.13
XLogP3:1
Hydrogen Bond Donor Count:1
Hydrogen Bond Acceptor Count:3
Rotatable Bond Count:2
Exact Mass:150.031694049
Monoisotopic Mass:150.031694049
Topological Polar Surface Area:54.4
Heavy Atom Count:11
Complexity:139
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes