叠氮化钠 → 5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrophenyl azide

HRID 463597笔记

反应方程式

HRID 463597 反应方程式
[Cl:1][C:2]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[C:7]([N+:14]([O-])=O)[CH:6]=1.[N-:25]=[N+:26]=[N-].[Na+]>CC(C)=O>[Cl:1][C:2]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[C:7]([N:14]=[N+:25]=[N-:26])[CH:6]=1

参与物

4

反应物 2

HCID 33557叠氮化钠HCID 156238Benzene, 2-chloro-1-(3,4-dinitrophenoxy)-4-(trifluoromethyl)-

产物 1

HCID 135053575-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrophenyl azide

试剂、催化剂与溶剂 1

HCID 180丙酮溶剂

实验过程

A mixture of 4-(2-chloro-4-trifluoromethylphenoxy)-1,2-dinitrobenzene (2.0 g, 5.5 mmol) and sodium azide (1.1 g, 16.6 mmol) in acetone (25 ml) is heated under reflux for 3.5 hours. The reaction is then cooled and filtered, and the filtrate is stripped. The residue is taken up in chloroform, washed with water (2X) and with brine, dried, stripped and purified by preparative thin layer chromatography (prep. TLC) (silica gel, eluting with 15% ethyl acetate/hexane) to give 5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrophenyl azide.

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 3.5 hours
  3. temperatureThe reaction is then cooled
  4. filtrationfiltered
  5. washwashed with water (2X) and with brine
  6. customdried
  7. custompurified by preparative thin layer chromatography (prep. TLC) (silica gel, eluting with 15% ethyl acetate/hexane)

来源与证据

ORD记录
ord-6be467e2eaa24931ab7484da4a7a0218
来源数据集
uspto-grants-1985_10
专利号
US04544400

反应笔记

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