4-Chlorobenzenesulfonyl chloride → HCID 14989646、化合物

HRID 1199685ノート

反応式

HRID 1199685 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[N:6][CH:7]=1.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([S:20](Cl)(=[O:22])=[O:21])=[CH:16][CH:15]=1>N1C=CC=CC=1>[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([S:20]([NH:1][C:2]2[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[N:6][CH:7]=2)(=[O:22])=[O:21])=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 149896425-amino-2-Pyridinepropanoic acid

生成物 1

HCID 14989646HCID 14989646、化合物収率 63.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 3-(5-aminopyrid-2-yl)propionic acid (1.00 g) and 4-chlorobenzenesulphonyl chloride (1.27 g) in pyridine (15 ml) was stirred at room temperature overnight. The solvent was removed and the residue was dissolved in dilute sodium hydroxide (30 ml) and extracted with chloroform (4×50 ml). The aqueous layer was acidified with dilute hydrochloric acid (pH 3) and extracted with ethyl acetate (4×100 ml). The ethyl acetate extracts were combined, dried over magnesium sulphate, the solvent was removed and the residue was recrystallised from acetonitrile to give the title compound (1.30 g). m.p. 144°-146° C.

後処理

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in dilute sodium hydroxide (30 ml)
  3. extractionextracted with chloroform (4×50 ml)
  4. extractionextracted with ethyl acetate (4×100 ml)
  5. dry with materialdried over magnesium sulphate
  6. customthe solvent was removed
  7. customthe residue was recrystallised from acetonitrile

出典と根拠

ORDレコード
ord-8bbe9c805f954f44b1889cc6e7c4ff1d
出典データセット
uspto-grants-1990_02
特許番号
US04902698

反応ノート

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