Hydrochloric Acid → 5-(2-Hydroxy-3,4-dimethoxyphenyl)isoindolin-1-one

HRID 2171017노트

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HRID 2171017 반응식
[CH3:1][O:2][C:3]1[C:4]([O:21]COC)=[C:5]([C:11]2[CH:12]=[C:13]3[C:17](=[CH:18][CH:19]=2)[C:16](=[O:20])[NH:15][CH2:14]3)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].Cl>CO>[OH:21][C:4]1[C:3]([O:2][CH3:1])=[C:8]([O:9][CH3:10])[CH:7]=[CH:6][C:5]=1[C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[C:16](=[O:20])[NH:15][CH2:14]2

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 674677335-(3,4-Dimethoxy-2-(methoxymethoxy)phenyl)isoindolin-1-one

생성물 1

HCID 674639885-(2-Hydroxy-3,4-dimethoxyphenyl)isoindolin-1-one

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

To a stirring solution of 5-(3,4-dimethoxy-2-(methoxymethoxy)phenyl)isoindolin-1-one (600 g, 1.81 mmol) in methanol (20 mL) at 0° C., was added concentrated hydrochloride acid (1 mL) and the resultant reaction mixture was stirred at 50° C. for 15 min. The reaction mixture was concentrated under reduced pressure and basified with aq sodium bicarbonate solution extracted with ethyl acetate (3×). The combined ethyl acetate layer was washed with brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure. Purification of the resulting residue by washings with ether afforded the title compound as a solid.

후처리

  1. customthe resultant reaction mixture
  2. concentrationThe reaction mixture was concentrated under reduced pressure and basified with aq sodium bicarbonate solution
  3. extractionextracted with ethyl acetate (3×)
  4. washThe combined ethyl acetate layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulphate
  6. concentrationconcentrated under reduced pressure
  7. customPurification of the resulting residue
  8. washby washings with ether

출처 및 근거

ORD 기록
ord-2f9a5bdac5904cf38b07246842438006
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051290B2

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