HRID379046

反应详情

EQUATION

反应方程式

HRID 379046 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 1-(4-cyano-3-fluorobenzyl)-5-(acetoxymethyl)imidazole hydrobromide (as described in Example 14, Step C) (31.87 g, 89.77 mmol) in 300 mL of 2:1 THF/water at 0° C. was added lithium hydroxide monohydrate (7.53 g, 179 mmol). After two hours, the reaction was concentrated in vacuo to a 100 mL volume, stored at 0° C. for 30 minutes, then filtered and washed with 700 mL of cold water to provide a brown solid. This material was dried in vacuo over P2O5 to provide the titled product as a pale brown powder which was sufficiently pure for use in the next step without further purification.

WORKUP

后处理

  1. concentrationthe reaction was concentrated in vacuo to a 100 mL volume
  2. waitstored at 0° C. for 30 minutes
  3. filtrationfiltered
  4. washwashed with 700 mL of cold water
  5. customto provide a brown solid
  6. dry with materialThis material was dried in vacuo over P2O5