HRID1085110

反应详情

EQUATION

反应方程式

HRID 1085110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 5-fluoro-2-mercapto-1H-benzimidazole (0.88 g, 0.0051 mol) in methanol (25 ml) NaOH (0.2 g, 0.0051 mol) dissolved in H2O (1 ml) and 4-cyclopropylmethoxy-2-chloromethyl-pyridine hydrochloride (0.91 g, 0.0046 mol) dissolved in methanol (10 ml) were added in the given order. The mixture was heated to boiling and NaOH (0.2 g, 0.005 mol) dissolved in H2O (1 ml) was added and the mixture was refluxed for 1 hour. After evaporation of methanol, CH2Cl2 (75 ml) and H2O (50 ml) were added and pH adjusted to 10. The mixture was vigorously stirred, the phases were separated, the organic phase was dried over Na2SO4 and evaporated giving the desired product (1.25 g, 72%). NMR data for the product is given below.

WORKUP

后处理

  1. additionwere added in the given order
  2. additionwas added
  3. temperaturethe mixture was refluxed for 1 hour
  4. customAfter evaporation of methanol, CH2Cl2 (75 ml) and H2O (50 ml)
  5. additionwere added
  6. customthe phases were separated
  7. dry with materialthe organic phase was dried over Na2SO4
  8. customevaporated