HRID1094460

反应详情

EQUATION

反应方程式

HRID 1094460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Acetic Acid Anhydride (17.9 mmol; 1.7 mL) was added to 3-Amino-2-picoline (17.0 mmol; 1.8 g) in dichloromethane (10 mL) and diisopropylethylamine (17.9 mmol; 3.1 mL) at 25° C. under argon. The reaction aged 30 min at 25° C. then was diluted with dichloromethane and extracted with water and brine. The aqueous layer was extracted with dichloromethane and ether then the combined organics were dried over sodium sulfate, filtered and concentrated in vacuo. The resulting yellow oil was purified by chromatography (0% to 66% ethyl acetate in hexane) to afford the title compound.

WORKUP

后处理

  1. extractionextracted with water and brine
  2. extractionThe aqueous layer was extracted with dichloromethane and ether
  3. dry with materialthe combined organics were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe resulting yellow oil was purified by chromatography (0% to 66% ethyl acetate in hexane)