HRID12490

反应详情

EQUATION

反应方程式

HRID 12490 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.5 mL concentrated aqueous HCl in 40 mL EtOH, acetophenone (30.0 g), paraformaldehyde (10.0 g) and dimethylamine hydrochloride (26.5 g) were added and the mixture was refluxed for 3 h. The mixture was cooled to room temperature, and the precipitate was filtered, washed with acetone and dried in vacuo to obtain 37.2 g of white crystalline material. 1H NMR (200 MHz, DMSO-d6) δ 2.84 (s, 6H), 3.38-3.55 (m, 2H), 3.57-3.74 (m, 2H), 7.48-7.73 (m, 3H), 7.97-8.10 (m, 2H).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 3 h
  2. filtrationthe precipitate was filtered
  3. washwashed with acetone
  4. customdried in vacuo