(p-Hydroxyphenyl)diphenylsulfonium trifluoromethanesulfonate → Cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt

HRID 2061305노트

반응식

HRID 2061305 반응식
FC(F)(F)S([O-])(=O)=O.[C:9]1([S+:15]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[Na].[F:30][C:31]([F:46])([S:42]([OH:45])(=[O:44])=[O:43])[CH2:32][O:33][C:34]([CH:36]1[CH2:41][CH2:40][CH2:39][CH2:38][CH2:37]1)=[O:35]>O>[C:9]1([S+:15]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[F:46][C:31]([F:30])([S:42]([OH:45])(=[O:44])=[O:43])[CH2:32][O:33][C:34]([CH:36]1[CH2:41][CH2:40][CH2:39][CH2:38][CH2:37]1)=[O:35]

참가 물질

4

반응물 2

HCID 22389942(p-Hydroxyphenyl)diphenylsulfonium trifluoromethanesulfonateHCID 87529755Cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester sodium salt

생성물 1

HCID 87529650Cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt수율 99%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

About 8 g of the diphenyl-4-hydroxyphenylsulfonium trifluoromethanesulfonate salt manufactured in the synthesis example 3 and about 9.05 g of a cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester sodium salt were dissolved in about 100 ml of an MC and about 100 ml of water, and a synthesis reaction (see Equation 12 below) was performed while strongly stirring for about three hours. In this instance, a process of the synthesis reaction was observed by 19F NMR using a small amount of an extracted organic phase. The organic phase was extracted when the synthesis reaction was terminated, and washed using the MC and hexane. Next, the solvents were removed, and drying under a reduced pressure was performed to obtain about 10.67 g (a yield: about 99%) of a cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt, and a structure of the cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt was observed by 1H-NMR (see FIG. 12):

후처리

  1. customa synthesis reaction (
  2. customIn this instance, a process of the synthesis reaction
  3. extractionThe organic phase was extracted when
  4. customthe synthesis reaction
  5. customwas terminated
  6. washwashed
  7. customNext, the solvents were removed
  8. customdrying under a reduced pressure

출처 및 근거

ORD 기록
ord-d2f9faf304494de6a400ea4f1a8fbde5
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08283102B2

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