HRID1165537

反应详情

EQUATION

反应方程式

HRID 1165537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of N-methyl-bis-(2-hydroxypropyl)amine (75g, 0.51 mol), trans-4-phenyl-3-buten-2-one (75g, 10.51 mol), ruthenium trichloride hydrate (0.626g 12.3 mmole), triphenylphosphine (2.0g 17.6 mmole), and tetraglyme (30g) was added to a 250-ml 3-neck round bottom flask connected with a fractional distillation set and a thermometer. The reaction was heated to 180° C. under nitrogen and the products were distilled out through the distillation set. The products (organic layer) were then fractionally distilled again to obtain a 65% yield of 3,4-dihydro-2,4,6-trimethyl-2H-1,4-oxazine.

WORKUP

后处理

  1. additionwas added to a 250-ml 3-neck round bottom flask
  2. distillationconnected with a fractional distillation
  3. distillationthe products were distilled out through the distillation
  4. distillationThe products (organic layer) were then fractionally distilled again