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Benzyl Bromide → 1-benzyl-5-(3,5-dichlorophenylthio)-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole

HRID 1415997
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HRID 1415997 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([S:9][C:10]2[NH:14][C:13]([CH2:15][O:16][CH2:17][C:18]3[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=3)=[N:12][C:11]=2[CH:26]([CH3:28])[CH3:27])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[CH2:29](Br)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.[OH-].[Na+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1>[CH2:29]([N:14]1[C:10]([S:9][C:4]2[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([Cl:8])[CH:5]=2)=[C:11]([CH:26]([CH3:28])[CH3:27])[N:12]=[C:13]1[CH2:15][O:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1
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참가 물질

6

반응물 3

HCID 7498Benzyl BromideHCID 14798Sodium HydroxideHCID 178491401HCID 178491401, 화합물

생성물 1

HCID 221309361-benzyl-5-(3,5-dichlorophenylthio)-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole수율 88%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매
HCID 8028
Tetrahydrofuran
용매

실험 절차

(1)In 10 ml of dry tetrahydrofuran was dissolved 423 mg (1.00 mmol)of 5-(3,5-dichlorophenylthio)-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole (16b), followed by addition of 205 mg (1.20 mmol)of benzyl bromide, 48 mg (1.2 mmol)of sodium hydroxide and 5 mg (0.015 mg)of tetrabutylammonium bromide at room temperature with stirring, and the mixture was stirred at the same temperature for 3 hours. This reaction mixture was concentrated under reduced pressure and the residue was diluted with water and extracted with methylene chloride. The organic layer was washed with water and dried over sodium sulfate. The solvent was distilled off under reduced pressure and the residual oil was fractionated by silica gel chromatography (ethyl acetate:methylene chloride=1:9). From the first fraction, 33 mg (yield 6.5%)of the objective position isomer (17f')was obtained. From the subsequent fraction, 450 mg (yield 88%) of 1-benzyl-5-(3,5-dichlorophenylthio)-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole (17f)was obtained.

후처리

  1. stirringthe mixture was stirred at the same temperature for 3 hours
  2. concentrationThis reaction mixture was concentrated under reduced pressure
  3. additionthe residue was diluted with water
  4. extractionextracted with methylene chloride
  5. washThe organic layer was washed with water
  6. dry with materialdried over sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure
  8. customFrom the first fraction, 33 mg (yield 6.5%)of the objective position isomer (17f')was obtained

출처 및 근거

ORD 기록
ord-c1890c22b24c4ac6ad67102c668cd28a
출처 데이터셋
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05910506

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