HRID628475
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customcautiously quenched by careful addition to saturated aqueous ammonium chloride solution
- customThe quenched reaction mixture
- extractionwas extracted with ethyl acetate
- customthe separated orgranic phase was dried
- concentrationconcentrated under vacuum