HRID1244156

反应详情

EQUATION

反应方程式

HRID 1244156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-t-Butoxycarbonylamino-4-hydroxymethyl-thiophene-3-carboxylic acid ethyl ester (2.83 g, 9.44 mmol) was dissolved in anhydrous CH2Cl2 (165 mL) and treated with manganese dioxide (16.41 g, 188.70 mmol). It was stirred at room temperature for 5 hr then it was filtered through a pad of Celite. The Celite was washed with copious amounts of acetone. The filtrate was concentrated in vacuo to give title compound (2.69 g, 95%). MS m/e (CI) 300.0 (M+H)+; 1H NMR (300 MHz, CDCl3): δ ppm 1.42 (t, 3H), 1.55 (s, 9H), 4.43 (q, 2H), 7.59 (s, 1H), 10.30 (s, 1H), 10.34 (s, 1H).

WORKUP

后处理

  1. filtrationit was filtered through a pad of Celite
  2. washThe Celite was washed with copious amounts of acetone
  3. concentrationThe filtrate was concentrated in vacuo