Toluene → HCID 135621797、化合物

HRID 846526

反応式

HRID 846526 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 135621797HCID 135621797、化合物収率 67.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-a4b596b4e33649ad8cef5419040e6c32
出典データセット
uspto-grants-1992_08
特許番号
US05136868

関連ノート

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