HRID1846816

反应详情

EQUATION

反应方程式

HRID 1846816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationthe mixture was concentrated in vacuo
  2. customThe residue was partitioned between saturated aqueous sodium bicarbonate solution and 10:1 DCM/MeOH the layers
  3. customwere separated
  4. extractionthe aqueous layer was extracted with 10:1 DCM/MeOH (3×)
  5. dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo