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Benzyl Bromide → Tert-butyl 4-(adamantan-2-yl(benzyloxy)methyl)-3-chlorobenzoate

HRID 1849750
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HRID 1849750 반응식
[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH:2]1[CH:11]([OH:26])[C:12]1[CH:24]=[CH:23][C:15]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])=[CH:14][C:13]=1[Cl:25])[CH2:8]2.[H-].[Na+].[CH2:29](Br)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>CN(C)C=O.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH:2]1[CH:11]([O:26][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:12]1[CH:24]=[CH:23][C:15]([C:16]([O:18][C:19]([CH3:21])([CH3:22])[CH3:20])=[O:17])=[CH:14][C:13]=1[Cl:25])[CH2:8]2
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참가 물질

6

반응물 3

HCID 7498Benzyl BromideHCID 24758Sodium hydrideHCID 86703631Tert-butyl 4-(adamantan-2-yl(hydroxy)methyl)-3-chlorobenzoate

생성물 1

HCID 86703632Tert-butyl 4-(adamantan-2-yl(benzyloxy)methyl)-3-chlorobenzoate수율 93.6%

시약·촉매·용매 2

HCID 67553Tetrabutylammonium Iodide촉매
HCID 6228
Dimethylformamide
용매

실험 절차

To a solution of tert-butyl 4-(adamantan-2-yl(hydroxy)methyl)-3-chlorobenzoate (0.32 mg, 1.00 mmol) in anhydrous dimethylformamide (5 mL) was added sodium hydride (60% dispersion in mineral oil, 0.048 g, 1.2 mmol) at 0° C. The reaction mixture was allowed to warm to ambient temperature and stirred for 1 hour. Benzyl bromide (0.24 mL, 2.00 mmol) and tetrabutylammonium iodide (0.037 g, 0.10 mmol) was added and the reaction mixture was stirred for 16 hours at ambient temperature. After quenched with saturated ammonium chloride solution (10 mL), the mixture was diluted with ethyl acetate (150 mL). The organic phase was washed with water (3×10 mL), brine (10 mL), dried over anhydrous sodium sulfate, and filtered. Concentration of the filtrate in vacuo gave a residue which was purified by silica gel column chromatography using 0-20% ethyl acetate in hexanes as eluent to afford the title compound as a colorless oil (0.437 g, quant.): 1H NMR (300 MHz, CDCl3) δ 7.97-7.95 (m, 1H), 7.90 (d, J=8.18 Hz, 1H), 7.60 (d, J=7.39 Hz, 1H), 7.46-7.18 (m, 5H), 5.18-5.11 (m, 1H), 4.30 (d, J=11.54 Hz, 1H), 4.18 (d, J=11.60 Hz, 1H), 2.41 (s, 1H), 2.12-1.30 (m, 22H), 1.13 (s, 1H).

후처리

  1. stirringthe reaction mixture was stirred for 16 hours at ambient temperature
  2. customAfter quenched with saturated ammonium chloride solution (10 mL)
  3. additionthe mixture was diluted with ethyl acetate (150 mL)
  4. washThe organic phase was washed with water (3×10 mL), brine (10 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customConcentration of the filtrate in vacuo gave a residue which
  8. customwas purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-845258253e874c0f8acd4b16190228cb
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952169B2

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