Chlorophenyl isocyanate → HCID 178518972、化合物

HRID 2226252ノート

反応式

HRID 2226252 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]=[C:9]=[O:10].C[Si]([N:15]=[N+:16]=[N-:17])(C)C>>[CH:5]1[CH:4]=[C:3]([N:8]2[NH:17][N:16]=[N:15][C:9]2=[O:10])[C:2]([Cl:1])=[CH:7][CH:6]=1

参加物

3

反応物 2

HCID 76833Chlorophenyl isocyanateHCID 78378Azidotrimethylsilane

生成物 1

HCID 178518972HCID 178518972、化合物収率 78.1%

実験手順

2-Chlorophenylisocyanate (7 g) and trimethylsilyl azide (7.9 g) were mixed and heated under refluxing for eight hours. The excessive trimethylsilyl azide was distilled off under reduced pressure and to the residue there were added 40 ml of methanol. Thereafter, the methanol was evaporated and the residue was purified by flush column chlomatography (hexane:ethyl acetate=2:1) to obtain the desired 1-(2-chlorophenyl)-5(4H)-tetrazolinone (7 g) having a melting point in the range of from 124.5° to 125.5° C.

後処理

  1. temperatureheated
  2. temperatureunder refluxing for eight hours
  3. distillationThe excessive trimethylsilyl azide was distilled off under reduced pressure and to the residue there
  4. additionwere added 40 ml of methanol
  5. customThereafter, the methanol was evaporated
  6. customthe residue was purified
  7. customby flush column chlomatography (hexane:ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-d4a2078f80cf4849ad577090be9300e4
出典データセット
uspto-grants-1994_09
特許番号
US05347010

反応ノート

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