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Hydrogen Bromide → 1-[(1R,2R)-3-bromo-1-ethyl-2-methylpropyl]-3-(phenylmethoxy)benzene

HRID 1771020
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인쇄 미리보기

반응식

HRID 1771020 반응식
[CH2:1]([C@@H:3]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:9]=1)[C@@H:4]([CH3:7])[CH2:5]O)[CH3:2].[BrH:22].O>ClCCl>[Br:22][CH2:5][C@H:4]([CH3:7])[C@H:3]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:9]=1)[CH2:1][CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 962WaterHCID 60164839(betaR,gammaR)-gamma-ethyl-beta-methyl-3-(phenylmethoxy)benzenepropanol

생성물 1

HCID 601648441-[(1R,2R)-3-bromo-1-ethyl-2-methylpropyl]-3-(phenylmethoxy)benzene수율 87%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The product of Example 32 (2.6 g, 9 mmol) was dissolved in dichloromethane, and the mixture was cooled in an ice-water bath, then 48% hydrobromic acid (0.54 mL, 10 mmol) was added dropwise, after the addition was complete, it was reacted at room temperature for 16 hours. After that, water was added therein for separating, the aqueous phase was extracted with dichloromethane three times, then the organic phases were combined, washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated to give the target compound 2.7 g, yield: 87%.

후처리

  1. temperaturethe mixture was cooled in an ice-water bath
  2. additionafter the addition
  3. customit was reacted at room temperature for 16 hours
  4. customfor separating
  5. extractionthe aqueous phase was extracted with dichloromethane three times
  6. washwashed with saturated brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f4751db056184ce698d8830437082d0b
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09249084B2

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