反应详情

温度

110 °C

To 2.28 g 4-(1-Ethyl-propylamino)-3-(2-pyrazol-1-yl-acetylamino)-benzoic acid methyl ester were added 50 ml of 4M hydrochloric acid in dioxane. Divided into five portions the reaction mixture was heated to 110° C. for 15 min in a microwave reactor. After cooling to the reaction mixture 6 ml of 10 M aqueous sodium hydroxide solution were added slowly. After 30 min at rt the reaction mixture was concentrated to a third of its volume and adjusted to pH 4 by the addition of 2M aqueous hydrochloric acid. It was extracted with ethyl acetate three times. The combined organic phases were dried over sodium sulphate and concentrated in vacuo. 1.86 g (90%) of 1-(1-Ethyl-propyl)-2-pyrazol-1-ylmethyl-1H-benzoimidazole-5-carboxylic acid were obtained.

1. additionwere added slowly
2. concentrationAfter 30 min at rt the reaction mixture was concentrated to a third of its volume
3. additionadjusted to pH 4 by the addition of 2M aqueous hydrochloric acid
4. extractionIt was extracted with ethyl acetate three times
5. dry with materialThe combined organic phases were dried over sodium sulphate
6. concentrationconcentrated in vacuo