HRID1016430
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 5.4 g of 1,2-phenylenediamine and 4.5 g of dihydro-furan-2-one in 50 mL of 4N hydrochloric acid was heated to reflux for 20 h, 1 teaspoon of decolorizing carbon added, and after another 15 min reflux, filtered hot. The filtrate was concentrated under reduced pressure to near dryness, the residue made basic (pH=8) with saturated sodium bicarbonate and extracted into 3×80 mL of ether. The combined extracts were dried over magnesium sulfate and concentrated under reduced pressure. After drying under vacuum, 8.4 g of 3-(1H-benzimidazol-2-yl)-propan-1-ol was obtained as a solid.
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux for 20 h
- addition1 teaspoon of decolorizing carbon added
- temperatureafter another 15 min reflux
- filtrationfiltered hot
- concentrationThe filtrate was concentrated under reduced pressure
- extractionextracted into 3×80 mL of ether
- dry with materialThe combined extracts were dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customAfter drying under vacuum