反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringThe reaction mixture was stirred at 60° C. for 2 hours
- concentrationconcentrated under reduced pressure
- customThe resulting residues were purified by silica gel column chromatography with system B as eluant