反应详情

The product of example 120 step (ii) (0.25 g) was dissolved in 1-methyl-2-pyrrolidinone (6 ml) and this solution was treated with 2-imidazolecarboxaldehyde (0.1 g) followed by acetic acid (0.13 g) and then sodium triacetoxyborohydride (0.37 g). the reaction mixture was stirred at room temperature for three days. At the end of this time the mixture was poured in to excess aqueous dilute hydrochloric acid, this solution was allowed to stand for 10 minutes before being basified by addition of excess aqueous sodium bicarbonate. The mixture was extracted with ethyl acetate, the organic layer was washed with water, dried and evaporated under reduced pressure. Purification was by chromatography eluting with methanol/chloroform (7/93). Yield 0.05 g as a solid.

1. waitto stand for 10 minutes
2. extractionThe mixture was extracted with ethyl acetate
3. washthe organic layer was washed with water
4. customdried
5. customevaporated under reduced pressure
6. customPurification
7. washeluting with methanol/chloroform (7/93)