HRID639197

反应详情

EQUATION

反应方程式

HRID 639197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

(2-Chloro-6-dimethylaminomethyl-naphthalen-1-yl)-acetic acid ethyl ester (223 mg, 0.73 mmol) is dissolved in dioxane (2.6 ml). Water (0.96 ml) and lithium hydroxide (21 mg, 0.88 mmol) are then added, and the reaction mixture is warmed to 60° C. for 4 h. HPLC analysis indicates complete conversion of starting material. The reaction is diluted with water, adjusted to pH 6-7 by addition of 1 M aqueous NaHSO4, and extracted with EtOAc. The water layer is then concentrated, and the solid residue is repeatedly extracted with MeOH to yield pure title compound. ES+-MS: 278.3, 280.1 [M+H]+.

WORKUP

后处理

  1. extractionextracted with EtOAc
  2. concentrationThe water layer is then concentrated
  3. extractionthe solid residue is repeatedly extracted with MeOH