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Carbon tetrabromide → 2-((5-(Bromomethyl)-2-methoxyphenoxy)methyl)-1,3-dimethylbenzene

HRID 337250
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반응식

HRID 337250 반응식
[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH2:14]O)[CH:9]=[CH:10][C:11]=1[O:12][CH3:13].C(Br)(Br)(Br)[Br:22].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[Br:22][CH2:14][C:8]1[CH:9]=[CH:10][C:11]([O:12][CH3:13])=[C:6]([CH:7]=1)[O:5][CH2:4][C:3]1[C:2]([CH3:1])=[CH:19][CH:18]=[CH:17][C:16]=1[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 66959381(3-(2,6-Dimethylbenzyloxy)-4-methoxyphenyl)methanol

생성물 1

HCID 669586602-((5-(Bromomethyl)-2-methoxyphenoxy)methyl)-1,3-dimethylbenzene

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of (3-(2,6-dimethylbenzyloxy)-4-methoxyphenyl)methanol (Step C, 5.23 g, 20.4 mmol) and CBr4 (10.16 g, 30.6 mmol) in dry CH2Cl2 (20 ml) was added portion wise triphenylphosphine (8.03 g, 30.64 mmol) at 0° C. The reaction mixture was stirred for 1.5 hours, filtered, concentrated and purified by flash chromatography on a silica gel column (hex: ethyl acetate 2:1) to give the title compound.

후처리

  1. filtrationfiltered
  2. concentrationconcentrated
  3. custompurified by flash chromatography on a silica gel column (hex: ethyl acetate 2:1)

출처 및 근거

ORD 기록
ord-c40a8a4e4f4b45ca8f2430e050286e3f
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889724B2

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