Hydrochloric Acid → HCID 21958032, 화합물

HRID 2299222노트

반응식

HRID 2299222 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][S:10]([CH:13]1[C:18]([C:19]([O:21][CH2:22][C:23]([O:25]C(C)(C)C)=[O:24])=[O:20])=[CH:17][CH2:16][CH2:15][CH2:14]1)(=[O:12])=[O:11].Cl>C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][S:10]([CH:13]1[C:18]([C:19]([O:21][CH2:22][C:23]([OH:25])=[O:24])=[O:20])=[CH:17][CH2:16][CH2:15][CH2:14]1)(=[O:12])=[O:11]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86758707HCID 86758707, 화합물2회

생성물 1

HCID 21958032HCID 21958032, 화합물수율 35.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

To a solution of t-butyl [6-[N-(2,4-difluorophenyl)sulfamoyl]-1-cyclohexen-1-yl]carbonyloxyacetate (Compound 59, 80 mg) obtained in Example 56 in ethyl acetate (4 ml), a 4N solution of hydrogen chloride in ethyl acetate (5 ml) was added with ice-cooling and the mixture was stirred at room temperature for 70 hours. The reaction mixture was evaporated under reduced pressure to dryness and the residue was purified by ODS column chromatography (eluent: methanol/water=3/2) to yield [6-[N-(2,4-difluorophenyl)sulfamoyl]-1-cyclohexen-1-yl]carbonyloxyacetic acid (Compound 60, 25 mg) as white powdery crystals.

후처리

  1. temperaturecooling
  2. customThe reaction mixture was evaporated under reduced pressure to dryness
  3. customthe residue was purified by ODS column chromatography (eluent: methanol/water=3/2)

출처 및 근거

ORD 기록
ord-27e50f150c9f4092a0574635a63dc291
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06495604B1

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