HRID1016430

反应详情

EQUATION

反应方程式

HRID 1016430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated
  2. temperatureto reflux for 20 h
  3. addition1 teaspoon of decolorizing carbon added
  4. temperatureafter another 15 min reflux
  5. filtrationfiltered hot
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. extractionextracted into 3×80 mL of ether
  8. dry with materialThe combined extracts were dried over magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customAfter drying under vacuum