Thionyl Chloride → 3-[3-(Chlorocarbonyl)benzene-1-sulfonyl]triaza-1,2-dien-2-ium-1-ide

HRID 267750노트

반응식

HRID 267750 반응식
[N:1]([S:4]([C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=1)[C:10](O)=[O:11])(=[O:6])=[O:5])=[N+:2]=[N-:3].S(Cl)([Cl:18])=O>>[N:1]([S:4]([C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=1)[C:10]([Cl:18])=[O:11])(=[O:6])=[O:5])=[N+:2]=[N-:3]

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 28289923-Azidosulfonylbenzoic acid

생성물 1

HCID 213906583-[3-(Chlorocarbonyl)benzene-1-sulfonyl]triaza-1,2-dien-2-ium-1-ide

반응 조건

온도
65 °C

실험 절차

11.3 grams (50 milimoles) of 3-(azidosulfonyl) benzoic acid and 31 grams (261 millimoles) of thionyl chloride were added to a 200 ml. round bottom flask equipped with a magnetic stirrer, nitrogen sparge, reflux condenser and heating mantle. The mixture was stirred for 3 hours at 65°C. and then the excess thionyl chloride was stripped under vacuum. A 75 per cent yield of 3-(azido-sulfonyl) benzoyl chloride was obtained and identified by spectroscopic analysis. Said benzoyl chloride was a straw-yellow liquid that slowly crystallized at room temperature and had a melting point of 41°C. and a refractive index of ND24.5 = 1.5751.

후처리

  1. customround bottom flask equipped with a magnetic stirrer
  2. customnitrogen sparge
  3. temperaturereflux condenser
  4. temperatureheating mantle

출처 및 근거

ORD 기록
ord-6679fd63614944eea6185ab5f552e1f8
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03944574

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