Hydrochloric Acid → (p-Hydroxyphenyl)diphenylsulfonium trifluoromethanesulfonate

HRID 2061301ノート

反応式

HRID 2061301 の反応式
[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

参加物

3

反応物 2

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

生成物 1

HCID 22389942(p-Hydroxyphenyl)diphenylsulfonium trifluoromethanesulfonate収率 71%

反応条件

温度
50 °C

実験手順

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):

後処理

  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

出典と根拠

ORDレコード
ord-3b879d908bfb4a72a1fab723f3821f72
出典データセット
uspto-grants-2012_10
特許番号
US08283102B2

反応ノート

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