HRID256123

反应详情

EQUATION

反应方程式

HRID 256123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 22.1 mmol of methyl 5-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)furo[3,2-b]pyridine-6-carboxylate in methanol is cooled to 0° C. and a few drops of methyl orange indicator added. The solution is stirred and treated with 22.1 mmol of concentrated hydrochloric acid. The solution is then treated with 22.1 mmol of sodium cyanoborohydride, and the pH maintained at ~3 by the addition of 2N methanolic HCl, stirred overnight, cooled to 0° C. and the pH of the solution adjusted to about 0 with HCl to decompose residual NaCNBH3. The pH is thereafter adjusted to 5-6 with 5N NaOH. The methanol is removed in vacuo and water added to dissolve inorganic salts. The mixture is extracted with CH2Cl2 and the extracts dried and concentrated to give the title compound.

WORKUP

后处理

  1. stirringstirred overnight
  2. customThe methanol is removed in vacuo and water
  3. additionadded
  4. dissolutionto dissolve inorganic salts
  5. extractionThe mixture is extracted with CH2Cl2
  6. customthe extracts dried
  7. concentrationconcentrated