3-Phenoxybenzyl alcohol → (2-Bromo-5-phenoxyphenyl)methanol

HRID 897511

반응식

HRID 897511 반응식
[O:1]([C:8]1[CH:9]=[C:10]([CH2:14][OH:15])[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:16]N1C(=O)CCC1=O>C(#N)C>[Br:16][C:11]1[CH:12]=[CH:13][C:8]([O:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:9][C:10]=1[CH2:14][OH:15]

참가 물질

4

반응물 2

HCID 262953-Phenoxybenzyl alcoholHCID 67184N-bromobutanimide

생성물 1

HCID 22346758(2-Bromo-5-phenoxyphenyl)methanol수율 85%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 3-phenoxyphenyl methanol (4.0 g, 0.020 mol) in anhydrous acetonitrile was added 1-bromo-2,5-pyrrolidinedione (3.73 g, 0.021 mol) at room temperature. The mixture was stirred at room temperature for one and a half hour under an atmosphere of nitrogen. The solvents were removed under the reduced pressure. Tetrachloromethane (100 mL) was added to the residue, and the mixture was filtered. The filtrate was concentrated into the residue, and the residue was purified by flash chromatography on silica gel using ethyl acetate/n-heptane (1:5) as mobile phase to yield (2-bromo-5-phenoxyphenyl)methanol (4.7 g, 0.017 mol):

후처리

  1. customThe solvents were removed under the reduced pressure
  2. additionTetrachloromethane (100 mL) was added to the residue
  3. filtrationthe mixture was filtered
  4. concentrationThe filtrate was concentrated into the residue
  5. customthe residue was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-4c6e8c4653174f90ad0e7c0236601317
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06921763B2

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