HRID1793992

反应详情

EQUATION

反应方程式

HRID 1793992 的结构方程式

PROCEDURE

实验过程

(10,11-Dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-10-yl)-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-methanone of Step B (0.300 g, 0.746 mmol) and 2,6-dimethyl-cyclohex-1-en-1-yl trifluoromethanesulfonate (0.255 g, 0.821 mmol) were reacted by the procedure described in Example 1, Step F. Purification by flash column chromatography on silica gel, eluting with a solvent gradient of from 30 to 60% ethyl acetate in hexane, followed by recrystallization from petroleum ether (−20° C.) afforded the title compound as white crystals, m.p. 153–154° C.

WORKUP

后处理

  1. customPurification by flash column chromatography on silica gel
  2. washeluting with a solvent gradient of from 30 to 60% ethyl acetate in hexane
  3. customfollowed by recrystallization from petroleum ether (−20° C.)