3-(METHYLAMINO)-1-PROPANOL

Colorless oil liquid

34b. 615.0 gr of a 40percent methylamine aqueous solution is added to a three-necked flask connected to a thermometer, cooled to 0 to 5 ° C, and 150.0 gr of 3-chloropropane-1-ol is slowly added thereto.When the addition is completed, the reaction solution is heated. After completion of the addition, the reaction mixture is stirred at 25 to 30 ° C for 17 hours and the filtrate is concentrated under reduced pressure to remove methylamine and aqueous solution.Distillation under reduced pressure at 45 to 48 ° C was carried out using a high vacuum pump (0.2 torr) to obtain 100.4 gr of 3- (N-methylamino) propan-1-ol. 100 g of the obtained 3- (N-methylamino) propan-1-ol was introduced into a three-necked flask connected to a thermometer at 0-5 DEG C with 380 g of 47percent HBr.When the addition is completed, the temperature of the reaction solution is raised, and water is continuously removed while keeping the temperature higher than 100 ° C.After removing a certain amount of water, 1600 mL of cold acetone is added, followed by heating to reflux. When the reaction solution becomes a clear solution, the solution is slowly cooled and crystallization proceeds.The mixture was further stirred at 0 ° C for 1 hour, filtered and dried to obtain 131.2 g of 3-bromo-N-methylpropanamine-bromate as a white solid.The 3-bromopropanol (10.0 g, 71 . 94 mmol) under cooling in ice dropping slowly added to the methylamine aqueous solution in (50 ml). After the completion of the dropping, the obtained mixture at the room temperature reaction 14 hours. Then obtained directly to the pressure of the concentrated to obtain yellow oily mixture (6.0 g), directly used for the next step reaction.General procedure: N-Alkylation reaction was performed in a volume of 500 ml stainless-steel autoclave batch reactor. A mixture of 2-aminoethanol (0.5 mol) with methanol (1.5 mol) was added to the reactor containing 4 wtpercent of catalyst (with respect to 2-aminoethanol). The N-alkylation reaction was conducted under the constant stirred with a speed 200 r min-1 at 220 °C and 4.3 MPa (To maintain thepressure in the reaction kettle by adding nitrogen) for 35 min. The reaction products were identified by GC'MS analysis (Agilent 5973N-6890N, Agilent Technologies). The selectivity and chemical conversions of the products were determined by GC analysis (GC-17A, Shimadzu Co; FID detector and DB-1 ms capillary column, J&W).

Molecular Weight:89.14
XLogP3:-0.5
Hydrogen Bond Donor Count:2
Hydrogen Bond Acceptor Count:2
Rotatable Bond Count:3
Exact Mass:89.084063974
Monoisotopic Mass:89.084063974
Topological Polar Surface Area:32.3
Heavy Atom Count:6
Complexity:23.5
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes