Tetraethyl ranelate

(1) In a 20 L autoclave, 1 kg of the compound of the formula (I), 12 L of tetrahydrofuran, 1.92 kg of potassium carbonate, 2.3 kg of ethyl bromoacetate, 20 g of crown ether were added and heated to reflux, HPLC control (Figure 9 for the end of the reaction HPLC control map), the reaction ended about 3-4h. Filter, filtrate vacuum distillation, 4L ethanol ice bath beating 3-4h, filter, filter cake with ice ethanol rinse, into the 45 oven, To obtain 1.25 kg of the compound of the formula (II) in a yield of 91percent and a purity of 99.86percent.Example 2(c): Ethyl 5-amino-4-cyano-3-(2-ethoxy-2-oxoethyl)-2-thiophene carboxylate (10 g) was added in acetone (70 ml) and water (3 ml) at ambient temperature followed by the addition of potassium carbonate (10.7 g), tetrabutyl ammonium iodide (2 g) and ethylchloro acetate (11.8 g) and reaction mass was heated to reflux for 3 hour. The reaction mass was cooled to ambient temperature. The reaction mass was filtered and washed with acetone (30 ml). The filtrate was concentrated under vacuum below 50°C. Ethanol (30 ml) was added to the concentrated mass and heated the reaction mixture till clear solution was obtained. Thereafter reaction mixture was cooled. The product was filtered and washed with ethanol (30 ml) and dried the product at 40- 50°C. Yield 91percent.(1) In a 20 L autoclave, 1 kg of the compound of the formula (I), 12 L of tetrahydrofuran, 1.92 kg of potassium carbonate, 2.3 kg of ethyl bromoacetate, 20 g of crown ether were added and heated to reflux, HPLC control (Figure 9 for the end of the reaction HPLC control map), the reaction ended about 3-4h. Filter, filtrate vacuum distillation, 4L ethanol ice bath beating 3-4h, filter, filter cake with ice ethanol rinse, into the 45 oven, To obtain 1.25 kg of the compound of the formula (II) in a yield of 91percent and a purity of 99.86percent.Example 2(c): Ethyl 5-amino-4-cyano-3-(2-ethoxy-2-oxoethyl)-2-thiophene carboxylate (10 g) was added in acetone (70 ml) and water (3 ml) at ambient temperature followed by the addition of potassium carbonate (10.7 g), tetrabutyl ammonium iodide (2 g) and ethylchloro acetate (11.8 g) and reaction mass was heated to reflux for 3 hour. The reaction mass was cooled to ambient temperature. The reaction mass was filtered and washed with acetone (30 ml). The filtrate was concentrated under vacuum below 50°C. Ethanol (30 ml) was added to the concentrated mass and heated the reaction mixture till clear solution was obtained. Thereafter reaction mixture was cooled. The product was filtered and washed with ethanol (30 ml) and dried the product at 40- 50°C. Yield 91percent.

Strontium ranelate intermediate.

Molecular Weight:454.5
XLogP3:3.1
Hydrogen Bond Acceptor Count:11
Rotatable Bond Count:16
Exact Mass:454.14098697
Monoisotopic Mass:454.14098697
Topological Polar Surface Area:161
Heavy Atom Count:31
Complexity:672
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes