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2-Bromopropane → 2-Bromo-1-isopropoxy-4-(trifluoromethoxy)benzene

HRID 1420808
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HRID 1420808 반응식
[Br:1][C:2]1[CH:7]=[C:6]([O:8][C:9]([F:12])([F:11])[F:10])[CH:5]=[CH:4][C:3]=1[OH:13].C([O-])([O-])=O.[K+].[K+].Br[CH:21]([CH3:23])[CH3:22].C(OCC)(=O)C>CN(C)C=O>[Br:1][C:2]1[CH:7]=[C:6]([O:8][C:9]([F:11])([F:12])[F:10])[CH:5]=[CH:4][C:3]=1[O:13][CH:21]([CH3:23])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 63582-BromopropaneHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 215840902-Bromo-4-(trifluoromethoxy)phenol

생성물 1

HCID 187825732-Bromo-1-isopropoxy-4-(trifluoromethoxy)benzene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-bromo-4-trifluoromethoxyphenol (Description 11; 1 g, 3.9 mmol) and K2CO3 (1.1 g, 7.8 mmol) in dimethylformamide (15 ml) was added 2-bromopropane (0.55 ml, 5.9 mmol). The solution was stirred for 14 h. at room temperature under an atmosphere of nitrogen. Waster (200 ml) and ethyl acetate (3×70 ml) was added to the solution and the organic phase washed with water (100 ml), brine (100 ml) and dried (MgSO4). The solvent was removed in vacuo and the residue purified by chromatography on silica gel (eluting with 5% ethyl acetate in hexane) to give the title compound. 1H NMR (250 MHz, CDCl3) δ1.38 (6H, d, J 6.1 Hz), 4.53 (1H, m), 6.88 (1H, d, J, 9 Hz), 7.12 (1H, dd, J 8.8, 2.6 Hz), and 7.43 (1H, d, J 2.8 Hz).

후처리

  1. washthe organic phase washed with water (100 ml), brine (100 ml)
  2. dry with materialdried (MgSO4)
  3. customThe solvent was removed in vacuo
  4. customthe residue purified by chromatography on silica gel (eluting with 5% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-52fcd8c4b6a54593af5c4724a2e8fd2c
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06071927

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