HRID1030579

反应详情

EQUATION

反应方程式

HRID 1030579 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-chloro-2-mercaptobenzimidazole (1.84 c, 10 mmol) (Varima, R. S., J. Indian Chem. Soc. 62, 73 (1985)) in methanol (10 mL) and 2N sodium hydroxide (13 mmol) was added octyl bromide (2.17 g, 10 mmol). The solution was stirred at ambient temperature for 72 hours, evaporated, dissolved in CH2Cl2, washed with brine and dried over Na2SO4. Evaporation of the solvent and flash chromatography (Merck Kieselgel, 5% Et2O/CH2Cl2) gave a residue which solidified on standing. A pentane wash gave the title compound as a beige solid (2.23 g), m.p. 66°-67° C. NMR (CDCl3)δ7.3(m, 3H), 5.33(t, J=6 Hz, 2H), 1.20(br, 15H).

WORKUP

后处理

  1. customevaporated
  2. dissolutiondissolved in CH2Cl2
  3. washwashed with brine
  4. dry with materialdried over Na2SO4
  5. customEvaporation of the solvent and flash chromatography (Merck Kieselgel, 5% Et2O/CH2Cl2)
  6. customgave a residue which
  7. washA pentane wash