4-Chlorobenzenesulfonyl chloride → HCID 14989646, 화합물

HRID 1199685노트

반응식

HRID 1199685 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 14989646HCID 14989646, 화합물수율 63.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8bbe9c805f954f44b1889cc6e7c4ff1d
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04902698

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