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Triphenylsulfonium chloride → Triphenylsulfonium (3-hydroxytricyclo[3.3.1.13,7]decane-1-methoxycarbonyl)difluoromethane sulfonate

HRID 333567
ノート
印刷プレビュー

反応式

HRID 333567 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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 75607088Triphenylsulfonium (3-hydroxytricyclo[3.3.1.13,7]decane-1-methoxycarbonyl)difluoromethane sulfonate

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-6194d96630784250b67e1d1aaadc07a8
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883394B2

反応ノート

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