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Carbon tetrabromide → 5-Bromo-2-(bromomethyl)-1,3-difluorobenzene

HRID 469829
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HRID 469829 반응식
[Br:1][C:2]1[CH:9]=[C:8]([F:10])[C:5]([CH2:6]O)=[C:4]([F:11])[CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:32]>C1COCC1>[Br:1][C:2]1[CH:9]=[C:8]([F:10])[C:5]([CH2:6][Br:32])=[C:4]([F:11])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 27733034-Bromo-2,6-difluorobenzyl alcohol

생성물 1

HCID 27733055-Bromo-2-(bromomethyl)-1,3-difluorobenzene

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a cooled (0° C.) solution of 4 g (17.6 mmol) 4-bromo-2,6-difluorobenzyl alcohol in 50 ml THF, 7 g (26.4 mmol) triphenylphosphine and 8.83 g (26.4 mmol) carbon tetrabromide are added with stirring. Stirring is continued for 10 min at 0° C. and for 1 h at room temperature. After that the reaction mixture is filtered and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, hexane) to afford the title compound as yellowish oil.

후처리

  1. additionare added
  2. stirringStirring
  3. filtrationAfter that the reaction mixture is filtered
  4. concentrationthe filtrate is concentrated in vacuo
  5. customThe residue is purified by chromatography (silicagel, hexane)

출처 및 근거

ORD 기록
ord-0d02b1b38e944b19896040d89c32db47
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08629168B2

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