反应详情

0.97 g (12.41 mmol) of sodium sulphide is added to a solution of 3.56 g (8.28 mmol) of the compound from Example 33A in 13 ml of dry DMF. The reaction mixture is stirred at +80° C. for 2 h. After cooling to RT, 2 ml of 37% strength hydrochloric acid are added to the reaction mixture, whose temperature rises to 65° C. After addition of 2.6 ml of water, the reaction mixture is cooled back to RT. After addition of a further 5 ml of water, the mixture is washed with 5 ml of ethyl acetate and made alkaline by addition of 40% strength sodium hydroxide solution. Yellow crystals precipitate, and these are filtered off with suction, washed with 10 ml of water and 10 ml of diethyl ether and then dried under reduced pressure. The filtrate is concentrated using a rotary evaporator and stirred with a little water. The resulting crystals are filtered off with suction, washed with in each case 10 ml of water and diethyl ether and dried under reduced pressure.

1. customrises to 65° C
2. temperaturethe reaction mixture is cooled back to RT
3. washthe mixture is washed with 5 ml of ethyl acetate
4. additionby addition of 40% strength sodium hydroxide solution
5. filtrationYellow crystals precipitate, and these are filtered off with suction
6. washwashed with 10 ml of water and 10 ml of diethyl ether
7. customdried under reduced pressure
8. concentrationThe filtrate is concentrated
9. customa rotary evaporator
10. stirringstirred with a little water
11. filtrationThe resulting crystals are filtered off with suction
12. washwashed with in each case 10 ml of water and diethyl ether
13. customdried under reduced pressure