Chlorophenyl isocyanate → HCID 178518972, 화합물

HRID 2226252노트

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HRID 2226252 반응식
[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

참가 물질

3

반응물 2

HCID 76833Chlorophenyl isocyanateHCID 78378Azidotrimethylsilane

생성물 1

HCID 178518972HCID 178518972, 화합물수율 78.1%

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d4a2078f80cf4849ad577090be9300e4
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05347010

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