HRID1846816
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
tert-Butyl 2-(trans-3-hydroxycyclobutyl)-1H-benzo[d]imidazole-1-carboxylate (0.31 g, 1.09 mmol) was stirred in a mixture of dichloromethane (5 mL) and TFA (5 mL) at RT for 4 h, then the mixture was concentrated in vacuo. The residue was partitioned between saturated aqueous sodium bicarbonate solution and 10:1 DCM/MeOH the layers were separated and the aqueous layer was extracted with 10:1 DCM/MeOH (3×). The combined extracts were dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo to give trans-3-(1H-benzo[d]imidazol-2-yl)cyclobutanol (0.11 g, 0.58 mmol, 54% yield) as a white solid.
WORKUP
后处理
- concentrationthe mixture was concentrated in vacuo
- customThe residue was partitioned between saturated aqueous sodium bicarbonate solution and 10:1 DCM/MeOH the layers
- customwere separated
- extractionthe aqueous layer was extracted with 10:1 DCM/MeOH (3×)
- dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo