HRID1109767

反应详情

EQUATION

反应方程式

HRID 1109767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 36 g of 6-methoxychroman-4-one and 290 ml of 48% hydrogen bromide solution in 290 ml of glacial acetic acid was heated to reflux for 3 hours. The solvent was removed in vacuo and the residue diluted with 2 l of water and stored in a refrigerator overnight. The resulting solid was filtered, washed with water and dried, 25.7 g. The original filtrate was extracted with ethyl acetate and the organic layer dried over sodium sulfate and concentrated to give an additional 4.75 g of the titled product.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 3 hours
  3. customThe solvent was removed in vacuo
  4. additionthe residue diluted with 2 l of water
  5. customstored in a refrigerator overnight
  6. filtrationThe resulting solid was filtered
  7. washwashed with water
  8. customdried
  9. extractionThe original filtrate was extracted with ethyl acetate
  10. dry with materialthe organic layer dried over sodium sulfate
  11. concentrationconcentrated