HRID37056

反应详情

EQUATION

反应方程式

HRID 37056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

5,9-Bis-(benzyloxymethyl)-l-oxa-4,7,10-triazacyclododecane-3,11-dione (0,250 g, 0,566 mmol) was dissolved in dry tetrahydrofuran (10 ml) cooled to 0° C. A 1M solution of borohydride-THF complex in tetrahydrofuran (5 ml) was added under nitrogen and the mixture was stirred at ambient temperature for 14 hours. 2M Hydrochloric acid (3 ml) was added and the mixture was concentrated in vacuo to approximately 1 ml volume. 25% Ammonia solution (2 ml) was added and the mixture was extracted four times with 4 ml of chloroform. The extracts were concentrated in vacuo and gave a yellow oil which showed an absence of carbonyl bands in IR. Yield 0,227 g (97%), FAB MS: 414(M+1).

WORKUP

后处理

  1. concentrationthe mixture was concentrated in vacuo to approximately 1 ml volume
  2. addition25% Ammonia solution (2 ml) was added
  3. extractionthe mixture was extracted four times with 4 ml of chloroform
  4. concentrationThe extracts were concentrated in vacuo
  5. customgave a yellow oil which