HRID2425527

反应详情

EQUATION

反应方程式

HRID 2425527 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To N-((trimethylsilyl)methyl)prop-2-en-1-amine (21 g, 146.5 mmol) was slowly added aqueous formaldehyde (20 g; 37% w/w) while stirring at room temperature. After 5 minutes additional stirring methanol (8 g) was added followed by the addition of K2CO3 (24 g). The reaction mixture was stirred overnight at room temperature. Water (100 ml) was added, followed by addition of tert-butyl methyl ether (75 ml). The organic layer was separated. The aqueous layer was extracted with tert-butyl methyl ether (75 ml). The combined organic extracts were dried with Na2SO4. Concentration under vacuum gave N-(methoxymethyl)-N-((trimethylsilyl)methyl)prop-2-en-1-amine as a clear oil (24 g, 128.1 mmol) in 87% c.y.

WORKUP

后处理

  1. additionwas added
  2. stirringThe reaction mixture was stirred overnight at room temperature
  3. customThe organic layer was separated
  4. extractionThe aqueous layer was extracted with tert-butyl methyl ether (75 ml)
  5. dry with materialThe combined organic extracts were dried with Na2SO4
  6. concentrationConcentration under vacuum