Water → Methyl [2-[(4-chlorophenyl)sulfonylamino]indan-5-yl]acetate

HRID 1612888ノート

反応式

HRID 1612888 の反応式
Cl.[NH2:2][CH:3]1[CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([CH2:12][C:13]([O:15][CH3:16])=[O:14])[CH:9]=2)[CH2:4]1.C(=O)([O-])[O-].[K+].[K+].O.[Cl:24][C:25]1[CH:30]=[CH:29][C:28]([S:31](Cl)(=[O:33])=[O:32])=[CH:27][CH:26]=1>C(OCC)(=O)C>[Cl:24][C:25]1[CH:30]=[CH:29][C:28]([S:31]([NH:2][CH:3]2[CH2:11][C:10]3[C:5](=[CH:6][CH:7]=[C:8]([CH2:12][C:13]([O:15][CH3:16])=[O:14])[CH:9]=3)[CH2:4]2)(=[O:33])=[O:32])=[CH:27][CH:26]=1

参加物

6

反応物 4

HCID 962WaterHCID 73984-Chlorobenzenesulfonyl chlorideHCID 11430Potassium CarbonateHCID 23359670Methyl (2-aminoindan-5-yl)acetate hydrochloride

生成物 1

HCID 53769737Methyl [2-[(4-chlorophenyl)sulfonylamino]indan-5-yl]acetate収率 79.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of methyl (2-aminoindan-5-yl)acetate hydrochloride (2.43 g), potassium carbonate (5.52 g), water (60 ml), ethyl acetate (60 ml) and 4-chlorophenylsulfonyl chloride (2.11 g) is stirred at room temperature for one hour. The ethyl acetate layer is separated from the reaction mixture, washed with aqueous saline solution, dried, and distilled under reduced pressure to remove the solvent. The resulting crude product is recrystallized from a mixture of ethyl acetate and n-hexane to give methyl [2-[(4-chlorophenyl)sulfonylamino]indan-5-yl]acetate (3.02 g).

後処理

  1. customThe ethyl acetate layer is separated from the reaction mixture
  2. washwashed with aqueous saline solution
  3. customdried
  4. distillationdistilled under reduced pressure
  5. customto remove the solvent
  6. customThe resulting crude product is recrystallized from a mixture of ethyl acetate and n-hexane

出典と根拠

ORDレコード
ord-c07939a770454ca5aeecac5a57acd48f
出典データセット
uspto-grants-1993_03
特許番号
US05190975

反応ノート

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