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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Sodium Thiosulfate → Trifluoroacetic acid

HRID 70711
ノート
印刷プレビュー

反応式

HRID 70711 の反応式
ClC1C=CC=[C:4]([C:8](OO)=O)[CH:3]=1.[CH:12]1([O:17][CH:18]([C:30]2[CH:35]=[CH:34][C:33](SC3CC3)=[CH:32][CH:31]=2)[C:19]2[NH:24][C:23](=[O:25])[C:22]([C:26]([F:29])([F:28])[F:27])=[CH:21][CH:20]=2)[CH2:16][CH2:15][CH2:14][CH2:13]1.[S:40]([O-:44])([O-])(=[O:42])=S.[Na+].[Na+].[C:47](=[O:50])(O)[O-:48].[Na+]>C(Cl)(Cl)Cl>[F:27][C:26]([F:29])([F:28])[C:47]([OH:48])=[O:50].[CH:12]1([O:17][CH:18]([C:30]2[CH:31]=[CH:32][C:33]([S:40]([CH:8]3[CH2:4][CH2:3]3)(=[O:44])=[O:42])=[CH:34][CH:35]=2)[C:19]2[NH:24][C:23](=[O:25])[C:22]([C:26]([F:29])([F:27])[F:28])=[CH:21][CH:20]=2)[CH2:16][CH2:15][CH2:14][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 58452349HCID 58452349、化合物

生成物 2

HCID 6422Trifluoroacetic acid収率 0.1%HCID 58452908HCID 58452908、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

3-Chloroperbenzoic acid (31 mg) was added to a solution of 6-{(cyclopentyloxy)[4-(cyclopropylsulfanyl)phenyl]methyl}-3-(trifluoromethyl)pyridin-2(1H)-one (25 mg) in chloroform (1 mL), and the mixture was stirred at room temperature overnight. A sodium thiosulfate solution and aqueous sodium bicarbonate were added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. The residue was purified by preparative HPLC (Waters Sunfire 19×150 mm 5 μm, rate: 20 mL/min, eluent: A=acetonitrile, B=0.1% trifluoroacetic acid solution, gradient: 10 to 90%) to give the title compound as a colorless amorphous (7 mg, 26%).

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customafter which the solvent was evaporated under reduced pressure
  4. customThe residue was purified by preparative HPLC (Waters Sunfire 19×150 mm 5 μm, rate

出典と根拠

ORDレコード
ord-01c13c1fe8664388bf3b8405f5196636
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822503B2

反応ノート

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