Hydrochloric Acid → 4-(2-hydroxy-3,4-dimethoxyphenyl)isobenzofuran-1(3H)-one

HRID 2171014노트

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HRID 2171014 반응식
[CH3:1][O:2][C:3]1[C:4]([O:21]COC)=[C:5]([C:11]2[CH:19]=[CH:18][CH:17]=[C:16]3[C:12]=2[CH2:13][O:14][C:15]3=[O:20])[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:19]=[CH:18][CH:17]=[C:16]2[C:12]=1[CH2:13][O:14][C:15]2=[O:20]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 674651214-(3,4-dimethoxy-2-(methoxymethoxy)phenyl)isobenzofuran-1(3H)-one

생성물 1

HCID 674665654-(2-hydroxy-3,4-dimethoxyphenyl)isobenzofuran-1(3H)-one

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

To a stirring solution of 4-(3,4-dimethoxy-2-(methoxymethoxy)phenyl)isobenzofuran-1(3H)-one (1.3 g, 3.9 mmol) in methanol (15 mL) at 0° C., was added concentrated hydrochloride acid (3 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 and purification. The resulting residue purified by washings with pentane to afford 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 and purification
  7. customThe resulting residue purified by washings with pentane

출처 및 근거

ORD 기록
ord-0e8de8e253dc47108ab3199bda8d7e07
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051290B2

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