反应详情

500 ml MDC was added in the residue of 3-(2-(benzyloxy)-5-bromophenyl)-3-phenylpropan-1-ol of formula (C) followed by the addition of 50.1 g triethyl amine at 25° C. to 35° C. Reaction mass was cooled to 20° C. to 25° C. followed by the addition of 48.96 g methane sulphonyl chloride. Temperature was raised to 25° C. to 30° C. and maintained for 30 minutes. Further, 300 ml water was added and reaction mass was cooled to 0° C. to 5° C. and pH adjusted to 2 to 3 using 20% hydrochloric acid solution. The reaction temperature was raised to 25° C. to 35° C. and stirred for 30 minutes. The layers were separated and to the MDC layer added 5 g of activated charcoal and stirred for 30 minutes. MDC was distilled out under vacuum below 50° C. and co-distil by 2×50 ml methanol. The residue was treated with 300 ml methanol and heated up to 60° C. to 65° C. and maintained for 1 hour. Further, reaction mass was cooled to 25° C. to 35° C. and further cooled to 0° C. to 5° C. Finally the product was washed with 2×50 ml chilled methanol and dried in hot air oven at 55° C. to 60° C. to afford the title compound 3-(2-(benzyloxy)-5-bromophenyl)-3-phenylpropyl methanesulfonate of formula (D).

1. customReaction mass
2. temperaturewas cooled to 20° C. to 25° C.
3. temperatureTemperature was raised to 25° C. to 30° C.
4. temperaturemaintained for 30 minutes
5. customreaction mass
6. temperaturewas cooled to 0° C. to 5° C.
7. temperatureThe reaction temperature was raised to 25° C. to 35° C.
8. customThe layers were separated and to the MDC layer
9. additionadded 5 g of activated charcoal
10. stirringstirred for 30 minutes
11. distillationMDC was distilled out under vacuum below 50° C. and co-distil by 2×50 ml methanol
12. additionThe residue was treated with 300 ml methanol
13. temperatureheated up to 60° C. to 65° C.
14. temperaturemaintained for 1 hour
15. customFurther, reaction mass
16. temperaturewas cooled to 25° C. to 35° C.
17. temperaturefurther cooled to 0° C. to 5° C
18. washFinally the product was washed with 2×50 ml
19. temperaturechilled methanol
20. customdried in hot air oven at 55° C. to 60° C.