HRID1896096

反应详情

EQUATION

反应方程式

HRID 1896096 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Refer to Journal of Organometallic Chemistry, 1985, 285(1-3), 293-303. Octacarbonyldicobalt (4.02 g, 11.76 mmol), ethyl chloroacetate (0.71 g, 5.88 mmol), potassium carbonate (1.62 g, 11.76 mmol) and 50 mL of methanol were added into the reaction flask. After stirring for 5 minutes, tert-butyl (R)-[3-oxo-1-(2,4,5-trifluoro-benzyl)-3-(1-bromo-3-trifluoromethyl-5,6-dihydro-8H-imidazo[1,5-a]pyrazin-7-yl)-prop yl]-carbamate 1n (2.3 g, 3.92 mmol) was added. The reaction mixture was stirred at 60° C. for 2 hours and then concentrated under reduced pressure. The resulting residues were purified by silica gel column chromatography with system B as eluant to obtain the title compound methyl (R)-7-[3-tert-butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyryl]-3-trifluoromethyl-5,6,7,8-tetrahydro-imidazo[1,5-a]pyrazine-1-formate 1p (1.1 g, yield 50%) as a white solid. MS m/z (ESI): 565.0 [M+1].

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at 60° C. for 2 hours
  2. concentrationconcentrated under reduced pressure
  3. customThe resulting residues were purified by silica gel column chromatography with system B as eluant