HRID2422396

反应详情

EQUATION

反应方程式

HRID 2422396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6 M hydrochloric acid (7 ml) was added to a solution of (8-benzyl-1,4-dioxaspiro[4,5]dec-8-yl)(4-methoxybenzyl)amine (1.2 g, 3.3 mmol) in acetone (17 ml). The reaction solution was stirred for 20 h at room temperature, then made alkaline (pH˜9) with 25% potassium carbonate solution and extracted with diethyl ether (3×20 ml). The combined organic phases were dried with sodium sulfate and concentrated to approx. 10 ml under vacuum. The precipitated deposit was filtered off and dried under vacuum. Yield: 790 mg (74%), white solid. Melting point: 122-124° C.

WORKUP

后处理

  1. extractionextracted with diethyl ether (3×20 ml)
  2. dry with materialThe combined organic phases were dried with sodium sulfate
  3. concentrationconcentrated to approx. 10 ml under vacuum
  4. filtrationThe precipitated deposit was filtered off
  5. customdried under vacuum