HRID1848561

反应详情

EQUATION

反应方程式

HRID 1848561 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 a solution of the product of Step J (340 mg, 0.723 mmol) in methylene chloride (30 mL) was added PCC (311 mg, 1.45 mmol) at 0° C. and the resulting solution was stirred at 0° C. for 2 h. The reaction mixture was partitioned between methylene chloride and saturated bicarbonate, and the alkaline phase was extracted with methylene chloride (3×50 mL). The combined organic phase was dried over sodium sulfate, concentrated and the residue was purified on TLC using 10% methanol/methylene chloride as developing solvents to give the title compound. LC/MS: (M+1)+: 469.20.

WORKUP

后处理

  1. customThe reaction mixture was partitioned between methylene chloride and saturated bicarbonate
  2. extractionthe alkaline phase was extracted with methylene chloride (3×50 mL)
  3. dry with materialThe combined organic phase was dried over sodium sulfate
  4. concentrationconcentrated
  5. customthe residue was purified on TLC