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Imidazole → Tert-butyl(2-fluoro-3-iodopropoxy)diphenylsilane

HRID 1847021
ノート
印刷プレビュー

反応式

HRID 1847021 の反応式
[Si:1]([O:18][CH2:19][CH:20]([F:23])[CH2:21]O)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I:24]I.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N1C=CN=C1.S([O-])([O-])(=O)=S.[Na+].[Na+]>ClCCl>[C:14]([Si:1]([O:18][CH2:19][CH:20]([F:23])[CH2:21][I:24])([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:16])([CH3:17])[CH3:15]
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 5

HCID 795ImidazoleHCID 807IodineHCID 11776TriphenylphosphineHCID 24477Sodium ThiosulfateHCID 579797963-((Tert-butyldiphenylsilyl)oxy)-2-fluoropropan-1-OL

生成物 1

HCID 86724949Tert-butyl(2-fluoro-3-iodopropoxy)diphenylsilane収率 58.4%

試薬・触媒・溶媒

1
HCID 6344Dichloromethane溶媒

実験手順

3-{[Tert-Butyl(diphenyl)silyl]oxy}-2-fluoropropan-1-ol(2.03 g, 6.12 mmol) was dissolved in dichloromethane (20 ml). Iodine (4.66 g, 18.36 mmol), triphenyl phosphine (4.82 g, 18.36 mmol) and imidazole (1.25 g, 18.36 mmol) were added to the solution under cooling on ice and the mixture was stirred at room temperature for 23 hours. A saturated sodium thiosulfate aqueous solution was added to the reaction solution under cooling on ice and stirred for a while, the solution was extracted with dichloromethane and the extract was dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to yield 1.58 g (58%) of the title compound in the form of a yellowish solid.

後処理

  1. temperatureunder cooling on ice
  2. temperatureunder cooling on ice
  3. stirringstirred for a while
  4. extractionthe solution was extracted with dichloromethane
  5. dry with materialthe extract was dried over anhydrous sodium sulfate
  6. customThe solvent was removed under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-e0a200a100564a9e8b9c815b1c2f1500
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952010B2

反応ノート

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