HRID348502

反应详情

EQUATION

反应方程式

HRID 348502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Bromo-1-(4-ethoxyphenyl)ethan-1-one (4.0 g) and N,N-bis(2-methylpropyl)-1-propenylamine (4.0 g) were added to 16 ml of dimethylacetamide under an atmosphere of nitrogen and the mixture was stirred between 50° C. and 55° C. for 2 hours. To the reaction mixture were added successively 1.6 g of paratoluenesulfonic acid and 2.1 g of neopentyl glycol and the mixture was stirred between 50° C. and 60° C. for 3 hours. After addition of 8 ml of water to the reaction mixture and cooling the reaction mixture to the room temperature, crystals precipitated. These crystals were isolated by filtration to give 3.7 g (yield 74%) of the title compound as white crystals. The 1H-NMR spectrum of the product is substantially identical with that of the product of Example 1.

WORKUP

后处理

  1. stirringthe mixture was stirred between 50° C. and 60° C. for 3 hours
  2. customprecipitated
  3. customThese crystals were isolated by filtration