HRID2173451

反应详情

EQUATION

反应方程式

HRID 2173451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-Methoxy-N-methyl-2,1,3-benzoxadiazole-5-carboxamide (630 mg, 3.04 mmol) in THF (5 mL) cooled to −40° C. was added methyl lithium solution (1.6M, 2.28 mL, 3.65 mmol). The reaction mixture was stirred at the same temperature for 1 h, then was quenched by addition of 1M HCl. The mixture was extracted with ethyl acetate and the organic layer was dried over MgSO4. Purification my flash chromatography afforded the title compound. 1H-NMR (500 MHz, CDCl3) δ ppm 8.48 (s, 1H), 8.02 (d, 1H), 7.91 (d, 1H), 2.72 (s, 3H).

WORKUP

后处理

  1. customwas quenched by addition of 1M HCl
  2. extractionThe mixture was extracted with ethyl acetate
  3. dry with materialthe organic layer was dried over MgSO4
  4. customPurification my flash chromatography