HRID67248

反应详情

EQUATION

反应方程式

HRID 67248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2,3-dihydro-3,3-dimethyl-2-morpholinobenzofuran-5-yl methanesulphonate (product of Example 2) (24.9 parts) in water (50 parts) and hydrochloric acid (22.4 parts) was rapidly heated to 90°-100° C. and then cooled after 2 minutes. The crude product was extracted into ether (3×60 parts) and the extracts washed with water (2×50 parts), dried with sodium sulphate and evaporated to leave a gum which crystallised to give 2,3-dihydro-3,3-dimethyl-2-hydroxybenzofuran-5-yl methanesulphonate, m.p. 69°-72° C. (16 parts)

WORKUP

后处理

  1. temperaturewas rapidly heated to 90°-100° C.
  2. temperaturecooled after 2 minutes
  3. extractionThe crude product was extracted into ether (3×60 parts)
  4. washthe extracts washed with water (2×50 parts)
  5. dry with materialdried with sodium sulphate
  6. customevaporated
  7. customto leave a gum which
  8. customcrystallised