HRID1809080

反应详情

EQUATION

反应方程式

HRID 1809080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Ethyl-thiophene-3-carboxylic acid ethyl ester (1.2 g, 6.52 mmol) was dissolved in acetic acid (10 mL). N-Bromosuccinimide (7.1 mmol) was added and the reaction was stirred for 4 hours. The solvent was removed under vacuum and the product purified by flash chromatography on silica, eluting with 0%-30% t-butylmethylether in cyclohexane. The fractions containing the desired product were concentrated under vacuum to give the title compound (0.7 g). 1H NMR (400 MHz, CHCl3-d): δ 7.05 (s, 1H), 4.3 (q, 2H), 2.75 (q, 2H), 1.4 (t, 3H), 1.3 (t, 3H).

WORKUP

后处理

  1. customThe solvent was removed under vacuum
  2. customthe product purified by flash chromatography on silica
  3. washeluting with 0%-30% t-butylmethylether in cyclohexane
  4. additionThe fractions containing the desired product
  5. concentrationwere concentrated under vacuum