HRID2225176

反应详情

EQUATION

反应方程式

HRID 2225176 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Preparation D10, Step 1: Butyryl chloride (0.68 mL, 6.5 mmol, 1 eq) was slowly dripped into a mixture of 2-amino-5-chlorobenzamide (1.10 g, 6.5 mmol, 1 eq), 1.000N NaOH (6.50 mL, 6.5 mmol, 1 eq) and THF (enough to dissolve) at 0° C. More acid chloride and base were added to drive the reaction to completion. After 4 days ethyl acetate was added followed by 1N HCl. The layers were separated and the organic layer washed with 1N HCl (2×), saturated sodium bicarbonate (1×), and brine (1×). The organic layer was dried (MgSO4) and stripped to yield 2-butyramido-5-chlorobenzamide (1.44 g) as a white powder. Mass Spec (ESI) (M+H)+=241.0.

WORKUP

后处理

  1. customPreparation D10, Step 1
  2. dissolutionto dissolve) at 0° C
  3. customthe reaction to completion
  4. customThe layers were separated
  5. washthe organic layer washed with 1N HCl (2×), saturated sodium bicarbonate (1×), and brine (1×)
  6. dry with materialThe organic layer was dried (MgSO4)