Sertraline Dimethyl Impurity HCl synthesis
- Product Name:Sertraline Dimethyl Impurity HCl
- CAS Number:122873-20-5
- Molecular formula:C18H19Cl2N
- Molecular Weight:320.26
Yield:122873-20-5 83%
Reaction Conditions:
with 18-crown-6 ether;carbon dioxide at 80; under 750.075 Torr; for 24 h;Inert atmosphere;Schlenk technique;Glovebox;
Steps:
7 Preparation of drug sertraline corresponding methylation product
1) Under the protection of nitrogen,In a glove box, 0.25 mmol sertraline,12 equivPMHS (3 mmol Si-H),10 mol% potassium phosphate, 20 mol% 18-crown-6, 1.6 ml acetonitrile were added to a 50 ml schlenk tube.2) through the double-tube in the liquid nitrogen cooling operation will be frozenThe N2 in the Schlenk tube is replaced with CO2 as the C1 source and the CO2 pressure is 1 bar.3) The reaction was carried out at 80 ° C for 72 hours.4) After the reaction was separated by column chromatography, the stationary phase was silica gel,The mobile phase is ethyl acetate.Bruker NMR,Finally, the corresponding methylation product of sertraline (as shown in FIG. 13 and FIG. 14) was obtained, yielding 83%.
References:
CN107337606,2017,A Location in patent:Paragraph 0085; 0086; 0087; 0088; 0089; 0090
