HRID346659

反应详情

EQUATION

反应方程式

HRID 346659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To 530 mg (1.0 mmol) of 4-[[(3-chloro-4-methoxyphenyl)methyl]amino]-6-cyano-3-quinolinecarboxylic acid pentafluorophenyl ester was added 15 mL of anhydrous DMF, and the resulting mixture was cooled to 0° C. A solution of 75 mg of NaBH4 in 5 mL of anhydrous DMF was added to the reaction mixture, resulting in a clear red solution with gas evolution. After stirring for 1 hour at 0° C., the reaction was quenched with 2% TFA/MeOH, and the solvent was removed under reduced pressure. The oily residue was purified by flash chromatography (silica gel, 3–5% MeOH/CH2Cl2) to afford 87 mg (25% yield) of the title compound. LC: 2.60′; MH+: 354.

WORKUP

后处理

  1. customresulting in a clear red solution with gas evolution
  2. customthe reaction was quenched with 2% TFA/MeOH
  3. customthe solvent was removed under reduced pressure
  4. customThe oily residue was purified by flash chromatography (silica gel, 3–5% MeOH/CH2Cl2)