Sodium Azide → 5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrophenyl azide

HRID 463597

反応式

HRID 463597 の反応式
[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

参加物

4

反応物 2

HCID 33557Sodium AzideHCID 156238Benzene, 2-chloro-1-(3,4-dinitrophenoxy)-4-(trifluoromethyl)-

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-6be467e2eaa24931ab7484da4a7a0218
出典データセット
uspto-grants-1985_10
特許番号
US04544400

関連ノート

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