Toluene → HCID 135621797, 화합물

HRID 846526

반응식

HRID 846526 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[O:10])=[C:4]([F:11])[CH:3]=1.[N:12]([Si](C)(C)C)=[N+:13]=[N-:14].C1(C)C=CC=CC=1>O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:9](=[O:10])[NH:14][N:13]=[N:12]2)=[C:4]([F:11])[CH:3]=1

참가 물질

5

반응물 3

HCID 1140TolueneHCID 78378AzidotrimethylsilaneHCID 45582034-Chloro-2-fluorophenyl isocyanate

생성물 1

HCID 135621797HCID 135621797, 화합물수율 67.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A stirred solution of 17.1 grams (0.10 mole) of 4-chloro-2-fluorophenyl isocyanate and 20.0 grams (0.17 mole) of azidotrimethylsilane was heated under reflux for 16 hours. The reaction mixture was cooled to ambient temperature and 60 ml of toluene and 100 ml of water were added. The mixture was allowed to stand for two hours and the resultant solid collected by filtration. The filter cake was washed with petroleum ether to yield 14.5 grams of 1-(4-chloro-2-fluorophenyl)-1,4-dihydro-5H-tetrazol-5-one; m.p. 185°-187° C. The reaction was repeated several times.

후처리

  1. temperatureunder reflux for 16 hours
  2. filtrationthe resultant solid collected by filtration
  3. washThe filter cake was washed with petroleum ether

출처 및 근거

ORD 기록
ord-a4b596b4e33649ad8cef5419040e6c32
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05136868

연결된 노트

불러오는 중…