HRID1653704

反应详情

EQUATION

反应方程式

HRID 1653704 的结构方程式

PROCEDURE

实验过程

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.5 g, 9.1 mmol) was dissolved in 1-propanol (30 ml). To the mixture was added thionyl chloride (1.1 g, 9.1 mmol) and the solution was refluxed for 22h. The solvent was evaporated in vacuo to dryness. The residue was crystallized from methanol/THF to give 1.06 g (56%) of white crystals, mp 128°-130° C. 300 MHz nmr indicated product. Microanalysis calc.: C 46.49, H 7.26, N 13.56, found: C 46.21, H 6.96, N 17.41.

WORKUP

后处理

  1. temperaturethe solution was refluxed for 22h
  2. customThe solvent was evaporated in vacuo to dryness
  3. customThe residue was crystallized from methanol/THF