HRID1498145

反应详情

EQUATION

反应方程式

HRID 1498145 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-[2-(2,2,2-trifluoro-ethyl)-2H-[1,2,4]triazol-3-yl]-4,5-dihydro-6-oxa-1,10b-diaza-benzo[e]azulene-9-carboxylic acid methyl ester (553 mg, 1.4 mmol) in dioxane (12.5 mL) and water (12.5 mL) was added lithium hydroxide (67 mg, 2.8 mmol) and the reaction mixture stirred at RT for 2 h. The reaction mixture was concentrated in vacuo to remove the dioxane and the resultant solution acidified to pH 1 by the addition of HCl (12 N). The precipitate formed was collected by filtration, washed with water and dried in vacuo at 40° C. to give the title compound (519 mg, 98%). LCMS: RT=4.04 min, M+H+=380

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customto remove the dioxane
  3. additionthe resultant solution acidified to pH 1 by the addition of HCl (12 N)
  4. customThe precipitate formed
  5. filtrationwas collected by filtration
  6. washwashed with water
  7. customdried in vacuo at 40° C.