huagongshe.com
HRID1391267

反应详情

EQUATION

反应方程式

HRID 1391267 的结构方程式

REACTANTS

反应物

2
结构：[N-]=[N+]=NCC(O)CN=[N+]=[N-]
HCID151367

1,3-Diazido-2-propanol

C3H6N6O

结构：O=C(Cl)CCC([N+](=O)[O-])([N+](=O)[O-])[N+](=O)[O-]
HCID12507556

未命名化合物

PRODUCTS

生成物

1
结构：[N-]=[N+]=NCC(CN=[N+]=[N-])OC(=O)CCC([N+](=O)[O-])([N+](=O)[O-])[N+](=O)[O-]
HCID12507557

未命名化合物

收率 73.5%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCCl
溶剂HCID11

1,2-Dichloroethane

C2H4Cl2

PROCEDURE

实验过程

A solution of 25g (0.1 mole) of 4,4,4-trinitrobutyryl chloride, 14.7g (0.1 mole) of 1,3-diazido-2-propanol, and 50 ml of ethylene dichloride was refluxed for one week. The solution was cooled, washed with water, dried, and concentrated to give 25.5g (73.5%) of amber liquid. The product was purified by dissolving in carbon tetrachloride and passing through a neutral alumina column. Concentration of this solution gave a yellow liquid, nD24 = 1.5029, d25 = 1.464. The infrared spectrum showed the expected strong absorption for azide (4.7μ), carbonyl (5.8μ), and nitro (6.2μ).

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. washwashed with water
  3. customdried
  4. concentrationconcentrated