HRID61200

反应详情

EQUATION

反应方程式

HRID 61200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of the product of Step 240a (99 mg, 0.216 mmol) and NH2NH2.H2O (43 mg, 0.864 mmol) in MeOH (10 mL) was heated to reflux for 2 h. The reaction mixture was cooled to rt then concentrated under reduced pressure. The resulting residue was purified by flash column chromatography on silica gel eluting with CH2Cl2/MeOH/conc. NH4OH (100:0:0 to 90:9:1) to afford the title compound as a white foam (33 mg, 45%). ESI MS (M+H) 329.

WORKUP

后处理

  1. temperatureto reflux for 2 h
  2. concentrationthen concentrated under reduced pressure
  3. customThe resulting residue was purified by flash column chromatography on silica gel eluting with CH2Cl2/MeOH/conc