HRID712651

反应详情

EQUATION

反应方程式

HRID 712651 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

(5-Bromo-pyridin-3-yl)-acetic acid (200 mg, 0.93 mmol), 2.0 M dimethylamine solution (0.93 mL, 1.9 mmol), HOBt (25 mg, 0.19 mmol) and triethylamine (0.38 mL, 2.8 mmol) are dissolved in 5.0 mL of DMF. Then 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (290 mg, 1.9 mmol) is added. The reaction mixture is stirred for 16 hrs before 30 mL of water and 30 mL of DCM are added. The aqueous layer is separated and extracted with DCM (4×10 mL). The organic layers are combined, dried and concentrated to give the crude product which is purified by flash chromatography to give 180 mg of 2-(5-bromo-pyridin-3-yl)-N,N-dimethyl-acetamide.

WORKUP

后处理

  1. additionare added
  2. customThe aqueous layer is separated
  3. extractionextracted with DCM (4×10 mL)
  4. customdried
  5. concentrationconcentrated
  6. customto give the crude product which
  7. customis purified by flash chromatography