HRID1081318

反应详情

EQUATION

反应方程式

HRID 1081318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringThis mixture was stirred for 15 minutes at room temperature
  2. concentrationwhich was then concentrated
  3. additionTo the concentrate was added ethyl acetate, which
  4. washwas washed with water
  5. customdried
  6. distillationthe solvent was distilled off