HRID328445

反应详情

EQUATION

反应方程式

HRID 328445 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Anhydrous potassium carbonate (11.04 g.) was added to a stirred suspension of N-hydroxyphthalimide (17.12 g.) in dry dimethyl sulphoxide (200 ml.). A brown colour developed, 2-chloromethylthiophene (28.5 g.) was added dropwise and the mixture was stirred for 16 hr., during which time the colour disappeared. The suspension was poured into water (800 ml.) and cooled to 5°. The white precipitate was filtered off, and recrystallised from ethanol to give colourless needles of N-(thien-2-ylmethoxy)phthalimide (23.4 g., 83%), m.p. 129.7°- 130.0° τ values (DMSO-d6) are 4.58 (CH2), 2.28, 2.68, 2.90 (thienyl protons), 2.08 (phthalimide protons).

WORKUP

后处理

  1. temperaturecooled to 5°
  2. filtrationThe white precipitate was filtered off
  3. customrecrystallised from ethanol