HRID77369

反应详情

EQUATION

反应方程式

HRID 77369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-amino-N-isopropylacetamide (11.3 g, 97.0 mmol) and N,N-diisopropylethylamine (20.1 g, 162 mmol) in dichloromethane (200 mL) was cooled using an ice water bath. A solution of 5-fluoro-2-nitrobenzoyl chloride (16.5 g, 81.0 mmol) in dichloromethane (200 mL) was added dropwise over 15 minutes. The resulting solution was stirred overnight. The reaction mixture was washed with 2N HCl solution (2×250 mL), brine (250 mL) and then dried over magnesium sulphate. The solution was filtered before concentrating under reduced pressure to afford 5-fluoro-N-(2-(isopropylamino)-2-oxoethyl)-2-nitrobenzamide (18.5 g, 65.0 mmol).

WORKUP

后处理

  1. washThe reaction mixture was washed with 2N HCl solution (2×250 mL), brine (250 mL)
  2. dry with materialdried over magnesium sulphate
  3. filtrationThe solution was filtered
  4. concentrationbefore concentrating under reduced pressure