HRID232337

反应详情

EQUATION

反应方程式

HRID 232337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
175 °C

PROCEDURE

实验过程

Formamide (4.0 g, 89 mmol), 2,2,4,4-tetramethyl-3-oxothietane (1.0 g, 6933 mmol) and boric acid (100 mg) were combined in a Teflon lined Parr bomb which was heated for 15 hours in a 175° C. oil bath. The reaction was cooled and the light brown mixture taken up in water (40 ml). The aqueous solution was extracted with methylene chloride (4×20 ml) and the combined extracts dried (MgSO4) and evaporated under reduced pressure to a light brown oil (1.02 g). The residue was hydrolyzed and the hydrolyzate worked up according to the procedure of Example 1 to give the title product 650 mg (65%), verified by its 1H-NMR spectrum.

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. extractionThe aqueous solution was extracted with methylene chloride (4×20 ml)
  3. dry with materialthe combined extracts dried (MgSO4)
  4. customevaporated under reduced pressure to a light brown oil (1.02 g)