HRID715522
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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A 5 mL microwave vial was charged with 1-{[(3S,5S)-5-methyl-1-oxaspiro[2.5]oct-5-yl]methyl}-1H-benzimidazole-6-carbonitrile (150 mg, 0.533 mmol),6-(ethyloxy)-3-pyridinamine (221 mg, 1.599 mmol) and MeOH (4 mL). The reaction mixture was stirred and heated to 120° C. for 24 h. The reaction mixture was concentrated down to afford an oil. The oil was purified by silica gel (40 g) loading and initially elluting in DCM through to 6% MeOH/DCM over 18 column volumes to afford 1-{[(1S,3S)-3-({[6-(ethyloxy)-3-pyridinyl]amino}methyl)-3-hydroxy-1-methylcyclohexaneyl]methyl}-1H-benzimidazole-6-carbonitrile as an colorless oil. MS (m/z) 420 (M+H+).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated down
- customto afford an oil
- customThe oil was purified by silica gel (40 g) loading