HRID1461714

反应详情

EQUATION

反应方程式

HRID 1461714 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8.4 g (0.023 mol) (Z)-2-[(diethoxyphosphinyl)amino]-α-(methoxyimino)-4-thiazoleacetic acid, ethyl ester, 9.25 ml (0.046 mol) 5N sodium hydroxide, 30 ml water, and 50 ml dioxane was stirred at room temperature for 18 hours. The solvent was evaporated, 30 ml of 50% saturated sodium chloride was added, the pH was adjusted to 4.5, and 3×30 ml ethyl acetate was added. The aqueous layer was then adjusted to pH 2.5, and extraction with ethyl acetate followed by evaporation yielded 4.6 g of a yellow oil; MS ((+) FAB), 338 (M+H); NMR (300 MHz, DCCl3) δ 1.36 (2t, 6, OCH2CH3), 4.01 (s, 3, OCH3), 4.18 (m, 4, OCH2), 7.10 (s, 1, thiazole H).

WORKUP

后处理

  1. customThe solvent was evaporated
  2. addition30 ml of 50% saturated sodium chloride was added
  3. additionwas added
  4. extractionThe aqueous layer was then adjusted to pH 2.5, and extraction with ethyl acetate
  5. customfollowed by evaporation