Hydrochloric Acid → (p-Hydroxyphenyl)diphenylsulfonium trifluoromethanesulfonate

HRID 2061301노트

반응식

HRID 2061301 반응식
[F:1][C:2]([F:8])([F:7])[S:3]([O-:6])(=[O:5])=[O:4].[C:9]1([S+:15]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:16]2[CH:21]=[CH:20][C:19]([O:22]COC)=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.Cl>>[F:1][C:2]([F:8])([F:7])[S:3]([O-:6])(=[O:5])=[O:4].[C:9]1([S+:15]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=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

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 49765819Diphenyl-4-methoxymethoxyphenylsulfonium trifluoromethanesulfonate salt

생성물 1

HCID 22389942(p-Hydroxyphenyl)diphenylsulfonium trifluoromethanesulfonate수율 71%

반응 조건

온도
50 °C

실험 절차

About 100 g of diphenyl-4-methoxymethoxyphenylsulfonium trifluoromethanesulfonate salt manufactured in the synthesis example 2 was mixed and stirred in about 300 ml of the MC, and about 548 ml of 6 N HCl aqueous solution was dropped and stirred at about 50° C. to perform a synthesis reaction (see Equation 3). Next, the synthesis reaction was terminated when the initiator on the TLC disappeared, and then the MC was added, and separation of phases was performed. Next, an organic phase was extracted, washed twice using brine, and dried using magnesium sulphate. Next, the organic phase was filtered and concentrated to obtain about 100 g (a yield: about 71%) of a diphenyl-4-hydroxyphenylsulfonium trifluoromethanesulfonate salt, and a structure of the diphenyl-4-hydroxyphenylsulfonium trifluoromethanesulfonate salt was observed by 1H-NMR (see FIG. 3):

후처리

  1. additionwas mixed
  2. additionwas dropped
  3. customa synthesis reaction (see Equation 3)
  4. customNext, the synthesis reaction
  5. customwas terminated when the initiator on the TLC
  6. additionthe MC was added
  7. customseparation of phases
  8. extractionNext, an organic phase was extracted
  9. washwashed twice using brine
  10. customdried
  11. filtrationNext, the organic phase was filtered
  12. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3b879d908bfb4a72a1fab723f3821f72
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08283102B2

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