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

HRID 259635노트

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HRID 259635 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-ide수율 75%

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온도
65 °C

실험 절차

11.3 grams (50 milimoles) of 3-(azidosulfonyl) benzoic acid and 31 grams (261 milimoles) 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 percent 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-d3d29db043de4b3ab69a877b22abf892
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04038456

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