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

HRID 463597

반응식

HRID 463597 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-6be467e2eaa24931ab7484da4a7a0218
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04544400

연결된 노트

불러오는 중…