反应详情

The product of example 148 step (i) (0.14 g) was stirred as a suspension in dichloromethane (4 ml) and to this mixture was added oxalyl chloride (0.05 g) followed by N,N-dimethylformamide (0.01 g). After stirring for 1 h at room temperature the mixture was treated with 2-aminocyanoacetanide (0.14 g) 1-methyl-2-pyrrolidinone (3 ml) and then N,N-diisopropylethylamine (1 ml), stirring was then continued for a further 18 h at room temperature. The reaction mixture was partitioned between aqueous sodium bicarbonate and ethyl acetate, the organic layer was washed with water, dried and evaporated under reduced pressure. Purification was by chromatography eluting with 25% ethyl acetate/isohexane. Yield 0.09 g as a solid.

1. waitwas then continued for a further 18 h at room temperature
2. customThe reaction mixture was partitioned between aqueous sodium bicarbonate and ethyl acetate
3. washthe organic layer was washed with water
4. customdried
5. customevaporated under reduced pressure
6. customPurification
7. washeluting with 25% ethyl acetate/isohexane