Triphenylsulfonium chloride → 912290-04-1

HRID 1404878

反応式

HRID 1404878 の反応式
[Na].[F:2][C:3]([F:23])([S:19]([OH:22])(=[O:21])=[O:20])[C:4]([O:6][CH2:7][C:8]12[CH2:17][CH:12]3[CH2:13][CH:14]([CH2:16][C:10]([OH:18])([CH2:11]3)[CH2:9]1)[CH2:15]2)=[O:5].[Cl-].[C:25]1([S+:31]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(Cl)(Cl)Cl>[OH:18][C:10]12[CH2:16][CH:14]3[CH2:13][CH:12]([CH2:17][C:8]([CH2:7][O:6][C:4]([C:3]([F:23])([F:2])[S:19]([O-:22])(=[O:20])=[O:21])=[O:5])([CH2:15]3)[CH2:9]1)[CH2:11]2.[C:38]1([S+:31]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=1

参加物

5

反応物 3

HCID 61343Triphenylsulfonium chlorideHCID 5360545SodiumHCID 577603663-Hydroxy-1-adamantylmethyl difluorosulfoacetate

生成物 1

HCID 75607088912290-04-1

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a obtained solution of the sodium salt of 3-hydroxy-1-adamantylmethyl difluorosulfoacetate, 17.2 parts of chloroform, and 2.9 parts of a 14.8 mass % aqueous triphenyl sulfonium chloride solution were added, and the mixture was stirred for 15 hours, and then an organic layer was separated from the resultant solution, and an aqueous layer was subjected to extraction with 6.5 parts of chloroform. Organic layers were combined and washed with an ion-exchanged water, and the obtained organic layer was concentrated. To the concentrated solution, 5.0 parts of tert-butyl methyl ether was added, and the resultant mixture was stirred and filtered to obtain, as a white solid, 0.2 parts of triphenylsulfonium 1-((3-hydroxy-1-adamantyl)methoxycarbonyl)difluoromethane sulfonate (B1-2).

後処理

  1. customan organic layer was separated from the resultant solution
  2. extractionan aqueous layer was subjected to extraction with 6.5 parts of chloroform
  3. washwashed with an ion-exchanged water
  4. concentrationthe obtained organic layer was concentrated
  5. additionTo the concentrated solution, 5.0 parts of tert-butyl methyl ether was added
  6. stirringthe resultant mixture was stirred
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-6352577f1c45465290f2269cd7033acd
出典データセット
uspto-grants-2014_12
特許番号
US08916330B2

関連ノート

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