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Methanol → HCID 69155736, 화합물

HRID 750250
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HRID 750250 반응식
Cl.[C:2]([C:5]1[CH:10]=[C:9]([CH2:11][O:12][C:13]([C:15]2[N:16]([CH2:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[C:17](=[O:32])[C:18]3[C:23]([C:24]=2[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[CH:22][C:21]([Br:31])=[CH:20][CH:19]=3)=[O:14])[CH:8]=[CH:7][N:6]=1)([OH:4])=[O:3].S(=O)(=O)(O)O.[CH3:45]O>>[CH3:45][O:3][C:2]([C:5]1[CH:10]=[C:9]([CH2:11][O:12][C:13]([C:15]2[N:16]([CH2:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[C:17](=[O:32])[C:18]3[C:23]([C:24]=2[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[CH:22][C:21]([Br:31])=[CH:20][CH:19]=3)=[O:14])[CH:8]=[CH:7][N:6]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 69157443HCID 69157443, 화합물

생성물 1

HCID 69155736HCID 69155736, 화합물

실험 절차

To a solution (3.0 ml) of 2-benzyl-6-bromo-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid 2-carboxypyridin-4-ylmethyl ester hydrochloride (120 mg) in methanol was added conc. sulfuric acid (0.3 ml) at 0° C. with stirring, and the mixture was stirred at 50° C. for 48 hrs. After cooling the mixture, the solvent was removed under reduced pressure. The residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate, and the organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by medium pressure preparative LC (hexane/ethyl acetate=4/1-1/1) to give the title compound (73 mg) as colorless crystals.

후처리

  1. stirringthe mixture was stirred at 50° C. for 48 hrs
  2. temperatureAfter cooling the mixture
  3. customthe solvent was removed under reduced pressure
  4. customThe residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate
  5. dry with materialthe organic layer was dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by medium pressure preparative LC (hexane/ethyl acetate=4/1-1/1)

출처 및 근거

ORD 기록
ord-1eb558143f5547edb0daa68ed75ffd11
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07402595B2

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