HRID916045

反应详情

EQUATION

反应方程式

HRID 916045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3-(2,3-Dihydrobenzofur-7-yl)-3-methylbutanoic acid (800 mg) in CH2Cl2 (10 mL) was treated with SOCl2 (0.315 mL) at 0° C. After 30 minutes, N,O-dimethylhydroxylamine hydrochloride (421 mg) in pyridine (1.5 mL) was added to the green mixture at 0° C. After another 30 minutes, 15 mL of 2 M HCl was added. The organic phase was separated and the aqueous layer was extracted with three 20 mL portions of CH2Cl2. The combined organic phases were dried over magnesium sulfate. The solvent was removed to yield 950 mg (99%) of 3-(2,3-dihydrobenzofur-7-yl)-3-methylbutanoic acid N,O-dimethylhydroxylamide as a yellowish oil.

WORKUP

后处理

  1. waitAfter another 30 minutes
  2. customThe organic phase was separated
  3. extractionthe aqueous layer was extracted with three 20 mL portions of CH2Cl2
  4. dry with materialThe combined organic phases were dried over magnesium sulfate
  5. customThe solvent was removed