3-Bromo-2-hydroxy-6-methoxybenzoic acid → 1-Bromo-4-methoxy-2-(methoxymethoxy)benzene

HRID 862347노트

반응식

HRID 862347 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[OH:10].BrC1C(O)=C([C:18]([O:21][CH3:22])=CC=1)C(O)=O>N1C2C(=CC=CC=2)C=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[O:10][CH2:18][O:21][CH3:22]

참가 물질

4

반응물 2

HCID 134938383-Bromo-2-hydroxy-6-methoxybenzoic acidHCID 134938392-Bromo-5-methoxyphenol

생성물 1

HCID 148270371-Bromo-4-methoxy-2-(methoxymethoxy)benzene

시약·촉매·용매 1

HCID 7047Quinoline용매

실험 절차

1-Bromo-2-hydroxy-4-methoxybenzene. 3-Bromo-2-hydroxy-6-methoxybenzoic acid [T. de Paulis et. al., J. Med. Chem., (1985), 28, 1263-1269] (5 g, 0.02 mol) was heated in quinoline (200 mL) at 160° C. for 1 h. On cooling, the product was partitioned between Et2O and 3M HCl. The organic extract was washed with water and brine then dried (MgSO4), filtered and evaporated to give the title compound which was recrystallized from 5% ethyl acetate/hexane (4 g, 97%); m.p. 40°-42° C. Anal. Calc. for C7H7BrO2 : C, 41.41; H, 3.48. Found C, 41.39; H, 3.37.

후처리

  1. temperatureOn cooling
  2. customthe product was partitioned between Et2O and 3M HCl
  3. extractionThe organic extract
  4. washwas washed with water and brine
  5. dry with materialthen dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-b229ba1c7cc745c7a538fe83f9726d27
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05716984

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