Potassium Carbonate → 5-[4-Difluoromethoxy-2-(3-hydroxy-2,2-dimethyl-propoxy)-3-methoxy-phenyl]-3H-isobenzofuran-1-one

HRID 2171084노트

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HRID 2171084 반응식
[F:1][CH:2]([F:23])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[C:12]3[C:16](=[CH:17][CH:18]=2)[C:15](=[O:19])[O:14][CH2:13]3)=[C:6]([OH:20])[C:5]=1[O:21][CH3:22].C(=O)([O-])[O-].[K+].[K+].Br[CH2:31][C:32]([CH3:36])([CH3:35])[CH2:33][OH:34]>C(#N)C>[F:23][CH:2]([F:1])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[C:12]3[C:16](=[CH:17][CH:18]=2)[C:15](=[O:19])[O:14][CH2:13]3)=[C:6]([O:20][CH2:31][C:32]([CH3:36])([CH3:35])[CH2:33][OH:34])[C:5]=1[O:21][CH3:22]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1425013-Bromo-2,2-dimethyl-1-propanolHCID 674684075-(4-(difluoromethoxy)-2-hydroxy-3-methoxyphenyl)isobenzofuran-1(3H)-one

생성물 1

HCID 674654735-[4-Difluoromethoxy-2-(3-hydroxy-2,2-dimethyl-propoxy)-3-methoxy-phenyl]-3H-isobenzofuran-1-one수율 8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
80 °C

실험 절차

To a stirring solution of 5-(4-(difluoromethoxy)-2-hydroxy-3-methoxyphenyl)isobenzofuran-1(3H)-one (100 mg, 0.31 mmol) in acetonitrile (10 mL) was added potassium carbonate (128 mg, 0.930 mmol) and 3-bromo-2,2-dimethyl-propan-1-ol (155 mg, 0.930 mmol) and the resultant reaction mixture was heated to 80° C. for 16 h. The reaction mixture was cooled to RT, filtered through celite and the filtrate was concentrated under reduced pressure. The residue was purified by prep TLC to afford title compound as a solid (10 mg, 8%).

후처리

  1. customthe resultant reaction mixture
  2. temperatureThe reaction mixture was cooled to RT
  3. filtrationfiltered through celite
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by prep TLC

출처 및 근거

ORD 기록
ord-1d790113a8274471a82cd275c70cb68e
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051290B2

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