HRID612303

反应详情

EQUATION

反应方程式

HRID 612303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-methyl-2-furoic acid (3.65 g, 28.97 mmol) in ethyl acetate (60 ml) was hydrogenated over 5% rhodium on carbon (250 mg) until hydrogen uptake ceased. The catalyst was filtered off and washed with ethyl acetate. The combined filtrates were concentrated in vacuo to yield the title compound as a pale yellow oil (3.67 g, 97%); νmax (CH2Cl2) 3384, 3359, 1775, 1724 and 1355 cm-1 ; δH (CDCl3, 250 MHz) 1.35 (3 H, d, J 6.1 Hz), 1.53 (1 H, m), 2.09 (1 H, m), 2.17-2.40 (2 H, m), 4.21 (1 H, m) and 4.46 (1 H, dd, J 8.9, 4.7 Hz). [Mass spectrum: +ve ion (ammonia) MNH4+ (148)].

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. washwashed with ethyl acetate
  3. concentrationThe combined filtrates were concentrated in vacuo