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Hydrogen Bromide → 5-Bromo-2-(bromomethyl)-1,3-difluorobenzene

HRID 858647
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HRID 858647 반응식
[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:9]O)=[C:6]([F:8])[CH:7]=1.[BrH:12].O>C(O)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:9][Br:12])=[C:6]([F:8])[CH:7]=1
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참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 962WaterHCID 27733034-Bromo-2,6-difluorobenzyl alcohol

생성물 1

HCID 27733055-Bromo-2-(bromomethyl)-1,3-difluorobenzene수율 98%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 5-Bromo-2-hydroxymethyl-1,3-difluoro-benzene (0.89 g, 4.0 mmol) and 30 wt % of hydrogen bromide in acetic acid was stirred at room temperature for 90 minutes before it was poured into 80 ml of water. The mixture was extracted with pentane (3×50 ml) and the combined organic layers were washed with water (3×20 ml), dried over MgSO4 and concentrated at low pressure to afford the desired product (10.0 g, 98% yield). 1H NMR (CDCl3) δ: 4.47 (s, 2H), 7.09–7.10 (m, 1H), 7.12–7.13 (m, 1H).

후처리

  1. extractionThe mixture was extracted with pentane (3×50 ml)
  2. washthe combined organic layers were washed with water (3×20 ml)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated at low pressure

출처 및 근거

ORD 기록
ord-ba6e6e5c48cd4d03884cbd039f21ad81
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07148226B2

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