Hydrochloric Acid → HCID 21958032、化合物

HRID 2299222ノート

反応式

HRID 2299222 の反応式
[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]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86758707HCID 86758707、化合物2 回

生成物 1

HCID 21958032HCID 21958032、化合物収率 35.9%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-27e50f150c9f4092a0574635a63dc291
出典データセット
uspto-grants-2002_12
特許番号
US06495604B1

反応ノート

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