Chlorophenyl isocyanate → HCID 178518972、化合物

HRID 260894ノート

反応式

HRID 260894 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 73.6%

実験手順

A mixture of 2-chlorophenylisocyanate (7 g) and trimethylsilyl azide (7.9 g) was refluxed under heating for either hours and then the mixture was evaporated to remove excess trimethylsilyl azide under reduced pressure distillation, followed by addition of methanol to the resulting residue. Thereafter, the methanol was distilled off under reduced pressure. The resulting residue was purified by flash column chromatography (eluent: hexane:ethyl acetate = 2:1) to obtain the desired 1-(2-chlorophenyl)-5(4H)-tetrazolinone (6.6 g) having a m.p. in the range of from 124° to 125.5° C., in a yield of 73% of theory.

後処理

  1. temperaturewas refluxed
  2. temperatureunder heating for either hours
  3. customthe mixture was evaporated
  4. customto remove excess trimethylsilyl azide
  5. distillationunder reduced pressure distillation
  6. additionfollowed by addition of methanol to the resulting residue
  7. distillationThereafter, the methanol was distilled off under reduced pressure
  8. customThe resulting residue was purified by flash column chromatography (eluent: hexane:ethyl acetate = 2:1)

出典と根拠

ORDレコード
ord-3fcef35fa0ee4454a3b1ad854e1a5147
出典データセット
uspto-grants-1996_06
特許番号
US05530135

反応ノート

読み込み中…