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HRID2208146

反应详情

EQUATION

反应方程式

HRID 2208146 的结构方程式

REACTANTS

反应物

2
结构：[N-]=[N+]=[N-].[Na+]
HCID33557

未命名化合物

结构：CC(C)(C)OC(=O)N[C@H]1CC[C@@H](OS(C)(=O)=O)C1
HCID86608906

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N[C@H]1CC[C@H](N=[N+]=[N-])C1
HCID86608905

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Crude product from example C4 is dissolved in dry DMF (180 mL). After addition of sodium azide (11.7 g; 180.0 mmol) the reaction mixture is stirred for three days at 60° C. After filtration the reaction mixture is concentrated under reduced pressure, diluted with dichloromethane, extracted with water, half saturated brine and dried over MgSO4. After column chromatography on silica gel (cyclohexane/AcOEt—9:1) 11.8 g of the title compound is obtained as pale yellow oil.

WORKUP

后处理

  1. filtrationAfter filtration the reaction mixture
  2. concentrationis concentrated under reduced pressure
  3. additiondiluted with dichloromethane
  4. extractionextracted with water, half saturated brine
  5. dry with materialdried over MgSO4