HRID628475

反应详情

EQUATION

反应方程式

HRID 628475 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NaH (1.2 g, 60% dispersion in mineral oil) was added to the product of Step A dissolved in diethyl carbonate (10 mL). The reaction mixture was stirred overnight and then cautiously quenched by careful addition to saturated aqueous ammonium chloride solution. The quenched reaction mixture was extracted with ethyl acetate, and the separated orgranic phase was dried and concentrated under vacuum to yield 2.1 g of the title compound containing approximately 30% diethyl carbonate. 1H NMR (CDCl3) δ 7.74 (s, 1H), 7.57 (d, 1H), 7.35-7.55 (m, 5H), 4.57 (s, 1H) 4.19 (q, 4H), 1.29 (t, 6H).

WORKUP

后处理

  1. customcautiously quenched by careful addition to saturated aqueous ammonium chloride solution
  2. customThe quenched reaction mixture
  3. extractionwas extracted with ethyl acetate
  4. customthe separated orgranic phase was dried
  5. concentrationconcentrated under vacuum