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Allyl bromide → HCID 22130396, 화합물

HRID 1857703
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HRID 1857703 반응식
[CH2:1]([O:8][CH2:9][C:10]1[NH:11][C:12]([S:18][C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)=[C:13]([CH:15]([CH3:17])[CH3:16])[N:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:26](Br)[CH:27]=[CH2:28].[OH-].[Na+]>O1CCCC1.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:28]([N:11]1[C:12]([S:18][C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)=[C:13]([CH:15]([CH3:17])[CH3:16])[N:14]=[C:10]1[CH2:9][O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[CH:27]=[CH2:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7841Allyl bromideHCID 14798Sodium HydroxideHCID 178440141HCID 178440141, 화합물

생성물 1

HCID 22130396HCID 22130396, 화합물수율 6.7%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 8028Tetrahydrofuran용매

실험 절차

In 10 ml of dry tetrahydrofuran was dissolved 744 mg (2.00 mmol) of 2-(benzyloxymethyl)-5-(3-chlorophenylthio)-4-isopropyl-1H-imidazole (16e), followed by addition of 410 mg (2.40 mmol) of allyl bromide, 96 mg (2.40 mmol) of sodium hydroxide and 5 mg (0.015 mg) of tetrabutylammoniumbromide at room temperature with stirring, and the mixture was stirred at room temperature for 3 hours. This reaction mixture was concentrated under reduced pressure, the residue was extracted with methylene chloride, the organic layer was washed with water arid dried over sodium sulfate. The solvent was concentrated under reduced pressure and the residual oil was fractionated by silica gel chromatography (ethyl acetate: methylene chloride=1:9). From the first fraction, 50 mg (yield 6.7%) of the objective position isomer (17g') was obtained, and then, 480 mg (yield 58%) of 1-allyl-2-benzyloxymethyl-5-(3-chlorophenylthio)-4-isopropyl-1H-imidazole (17g) was obtained.

후처리

  1. stirringthe mixture was stirred at room temperature for 3 hours
  2. concentrationThis reaction mixture was concentrated under reduced pressure
  3. extractionthe residue was extracted with methylene chloride
  4. washthe organic layer was washed with water arid
  5. dry with materialdried over sodium sulfate
  6. concentrationThe solvent was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-443df21f929e4bdeaedae7099eb15d1a
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06147097

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