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Sodium Thiosulfate → HCID 90047349、化合物

HRID 1507560
ノート
印刷プレビュー

反応式

HRID 1507560 の反応式
[F:1][C:2]1[C:3]([Si](C)(C)C)=[CH:4][CH:5]=[C:6]2[C:10]=1[N:9]([CH3:11])[C:8](=[O:12])[C:7]2([CH3:14])[CH3:13].[I:19]Cl.S([O-])([O-])(=O)=S.[Na+].[Na+]>ClCCl>[F:1][C:2]1[C:3]([I:19])=[CH:4][CH:5]=[C:6]2[C:10]=1[N:9]([CH3:11])[C:8](=[O:12])[C:7]2([CH3:14])[CH3:13]
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 24477Sodium ThiosulfateHCID 24640Iodine chlorideHCID 90046406HCID 90046406、化合物

生成物 1

HCID 90047349HCID 90047349、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 7-fluoro-1,3,3-trimethyl-6-(trimethylsilyl)indolin-2-one (9.9 g, 37.3 mmol) in dichloromethane (500 ml) at 0° C. was added iodine monochloride (37.3 ml, 37.3 mmol). The reaction mixture was warmed to room temperature and stirred for 16 hours. A saturated aqueous solution of sodium thiosulfate was added to the reaction mixture and the aqueous phase was extracted with dichloromethane. The combined organic layers were dried over sodium sulfate. The solvent was evaporated and the residue purified by silica gel chromatography using ethyl acetate/heptane as eluent. The title compound was obtained as off-white crystals (9.82 g).

後処理

  1. extractionthe aqueous phase was extracted with dichloromethane
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. customThe solvent was evaporated
  4. customthe residue purified by silica gel chromatography

出典と根拠

ORDレコード
ord-885dffb7df454b93a87cef7ac9072069
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09221816B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート