反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of the compound (310 mg) obtained in Example 29 in methanol (15 ml) was added portionwise sodium borohydride (50 mg) at room temperature while stirring. This mixture was stirred for 15 minutes at room temperature, which was then concentrated. To the concentrate was added ethyl acetate, which was washed with water and dried, then the solvent was distilled off to leave N-[3,5-bis(trifluoromethyl)benzyl]-5-(4-fluorophenyl)-1,2,7,8-tetrahydro-N,1,7-trimethyl-8-oxo-6-pyrido[3,4-b]pyridinecarboxamide as a pale yellow oily product [NMR (200 MHz,CDCl3) ppm: 2.70(3H,s), 3.16(3H,s), 3.49(3H,s), 3.49(1H,m), 3.88(1H,m), 4.29(1H,d,J=14.6 Hz), 4.66(1H,d,J=14.6 Hz), 5.62(1H,m), 5.77(1H,d,J=13 Hz), 6.84-7.26(4H,m), 7.53(2H,s), 7.81(1H,s)].
WORKUP
后处理
- stirringThis mixture was stirred for 15 minutes at room temperature
- concentrationwhich was then concentrated
- additionTo the concentrate was added ethyl acetate, which
- washwas washed with water
- customdried
- distillationthe solvent was distilled off