HRID532900

反应详情

EQUATION

反应方程式

HRID 532900 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)ethanone (81.0 g, 230 mmol) and DMF-DMA (77.0 mL, 575 mmol) in MeOH (500 mL) was heated to reflux for 72 h. The mixture was then allowed to cool to RT and was then cooled to 0° C. the suspension was filtered and the filter cake was dried in vacuo at 40° C. to give the title compound (72.7 g) that was used as it is in the next step. UPLC-MS: MS 408.3 (M+H+); UPLC rt 1.08 min.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 72 h
  3. temperaturewas then cooled to 0° C. the suspension
  4. filtrationwas filtered
  5. customthe filter cake was dried in vacuo at 40° C.