HRID1107257

反应详情

EQUATION

反应方程式

HRID 1107257 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 title compound of Example 11, Step A (771 mg, 1-80 mmol) in dichloromethane (10 mL) was added dropwise diethylaminosulfur trifluoride (0.48 mL, 3.60 mmol) at 0° C. The reaction was stirred at 0° C. for 1 hour, quenched with cold water, and extracted with dichloromethane. The combined organic layers were washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The title compound of Step A, a compound of this invention, was isolated by flash chromatography (332 mg) as a foam melting at 60-64° C. 1H NMR (CDCl3) 87.7 (d, 1H), 7.4 (d, 1H), 7.1 (br s, 1H), 5.28 and 5.12 (two br s, 1 H), 4.6 (s, 2H), 1H), 4.2 (dd, 1H), 3.3 (ddd, 1H), 2.65 (m, 1H), 2.2 (m, 1H), 1.9-1.6 (m, 2H).

WORKUP

后处理

  1. customquenched with cold water
  2. extractionextracted with dichloromethane
  3. washThe combined organic layers were washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure