HRID131576

反应详情

EQUATION

反应方程式

HRID 131576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product of example 3 part b) (0.5 g, 1.28 mmol), 2-chlorobenzimidazole (0.21 g, 1.37 mmol), potassium carbonate (0.36 g, 2.6 mmol) and DMF (10 ml) were stirred for 1.5 h. Ethyl acetate and water were added to the reaction mixture. The two phases were separated, the organic layer was dried (MgSO4) and then concentrated in vacuo. The residue was purified by biotage eluting with dichloromethane to give the sub-title compund as a pale yellow solid, 0.36 g (61%). δ 1HD6DMSO 0.83 and 0.91 (6H, d), 2.1-2.22 (1H,m), 3.38 (3H,s), 3.67 (2H,d), 4.1 (3H,s), 5.58 (2H,s), 7.26-7.38 (2H,m), 7.41-7.48 (1H,m) and 7.7-7.8 (1H,m).

WORKUP

后处理

  1. customThe two phases were separated
  2. dry with materialthe organic layer was dried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by biotage
  5. washeluting with dichloromethane
  6. customto give the sub-title compund as a pale yellow solid, 0.36 g (61%)