HRID1095274

反应详情

EQUATION

反应方程式

HRID 1095274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7a (0.80 g, 2.2 mmol) and iodine (20 mg) in DMSO (5 ml) was refluxed for 1 h, and then carefully poured onto crushed ice. The precipitate was filtered and washed with 20% Na2SO3. Recrystallization of the precipitate from acetone afforded 8 (0.73 g, 93%). 1H NMR (400 MHz, CDCl3) δ 3.91 (s, 3H), 3.97 (s, 3H), 3.98 (s, 3H), 6.74 (s, 1H), 6.82 (s, 1H), 8.03 (d, J=8.8 Hz, 2H), 8.34 (d, J=8.8 Hz, 2H).

WORKUP

后处理

  1. temperaturewas refluxed for 1 h
  2. additioncarefully poured
  3. customonto crushed ice
  4. filtrationThe precipitate was filtered
  5. washwashed with 20% Na2SO3
  6. customRecrystallization of the precipitate from acetone