HRID532903

反应详情

EQUATION

反应方程式

HRID 532903 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(1-trityl-1H-imidazol-4-yl)cyclopropanol (2.4 g, 6.55 mol) was treated with a 90% aq. solution of formic acid (50 mL) and the mixture was stirred at RT for 24 h. The mixture was then concentrated in vacuo, diluted in a small volume of MeOH, and the solution was rendered basic with a 7M solution of NH3 in MeOH. The white precipitate was filtered off and the filtrate was concentrated in vacuo. Purification by flash chromatography (SiO2, DCM/MeOH 100:0 to 85:15) afforded the title compound (920 mg). UPLC-MS: MS 125.1 (M+H+).

WORKUP

后处理

  1. concentrationThe mixture was then concentrated in vacuo
  2. additiondiluted in a small volume of MeOH
  3. filtrationThe white precipitate was filtered off
  4. concentrationthe filtrate was concentrated in vacuo
  5. customPurification by flash chromatography (SiO2, DCM/MeOH 100:0 to 85:15)