Phenoxathiin → 10-Phenyl-10-phenoxathiinium methylsulfate

HRID 529870

반응식

HRID 529870 반응식
[CH:1]1[C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[O:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH3:15][O:16][S:17]([O-:20])(=[O:19])=[O:18].[C:21]1([I+]C2C=CC=CC=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C([O-])(=O)C1C=CC=CC=1.[Cu+2].C([O-])(=O)C1C=CC=CC=1.ClC1C=CC=CC=1>[CH3:15][O:16][S:17]([O-:20])(=[O:19])=[O:18].[C:21]1([S+:13]2[C:14]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=3[O:6][C:7]3[C:12]2=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

참가 물질

5

반응물 2

HCID 9217PhenoxathiinHCID 131735634Diphenyliodonium methylsulfate

생성물 1

HCID 13173563310-Phenyl-10-phenoxathiinium methylsulfate수율 63%

시약·촉매·용매 2

HCID 164650Cupric benzoate촉매HCID 7964Chlorobenzene용매

반응 조건

온도
120 °C

실험 절차

A mixture of 20 g of phenoxathiin, 43.1 g of diphenyliodonium methylsulfate, 0.9 g of copper(II) benzoate, and 210 g of chlorobenzene was heated and stirred at 120° C. for 3 hours. The reaction solution was cooled to room temperature and combined with 20 g of diisopropyl ether for crystallization. The solid was dried under reduced pressure, obtaining the target compound, 10-phenyl-10-phenoxathiinium methylsulfate. Amount 24.7 g, yield 63%.

후처리

  1. temperaturewas heated
  2. temperatureThe reaction solution was cooled to room temperature
  3. customcombined with 20 g of diisopropyl ether for crystallization
  4. customThe solid was dried under reduced pressure

출처 및 근거

ORD 기록
ord-7ef7710bf9914b4bab93fe308ab8d136
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09348227B2

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