HRID1707172

反应详情

EQUATION

反应方程式

HRID 1707172 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of ethyl thien-3-yl-glyoxylate (10 g) and 2 N-sodium hydroxide (50 ml) was added sufficient methanol to produce a homogeneous solution, and the reaction was allowed to stand at room temperature for one hour. The solution was poured into water, extracted with ether, acidified with 2 N-hydrochloric acid and extracted with ether. The combined extracts were dried and evaporated to give an oil which was triturated with benzene-petroleum ether, and the resulting solid filtered and dried (7.5 g; 88%), m.p. 63°, νmax. (Nujol) 3600 and 1702 cm-1 (CO2H), τ (DMSO-d6) values include 1.29, 2.21, 2.38 (thien-3-yl protons).

WORKUP

后处理

  1. customto produce a homogeneous solution
  2. extractionextracted with ether
  3. extractionextracted with ether
  4. customThe combined extracts were dried
  5. customevaporated
  6. customto give an oil which
  7. customwas triturated with benzene-petroleum ether
  8. filtrationthe resulting solid filtered
  9. customdried (7.5 g; 88%), m.p. 63°, νmax