HRID479287

反应详情

EQUATION

反应方程式

HRID 479287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2 g (14 mmole) of methyl-3-methoxy-5-trifluoromethyl-2-thiophenecarboxylate, 2 g (28 mmole) of KOH in a mixture of 15 mL water and 50 mL of methanol was refluxed for 2 hr. The reaction mixture was partitioned with ether and dilute aqueous HCl. The organic phase was separated, dried over MgSO4, filtered and concentrated to give 2.8 g (87%) of a colorless solid. mp 131-132° C. 1H NMR (300 MHz, CDCl3): δ 7.2 (s, 1H); 4.1 (s, 3H). Anal. Calc'd for C7H5F3O3S: C, 37.17; H, 2.23; S, 14.18. Found: C, 36.96; H, 2.19; S, 14.08.

WORKUP

后处理

  1. temperaturewas refluxed for 2 hr
  2. customThe reaction mixture was partitioned with ether and dilute aqueous HCl
  3. customThe organic phase was separated
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated