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Pyrrolidine-1-carbonitrile → HCID 178454466, 화합물

HRID 1418851
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HRID 1418851 반응식
[ClH:1].[CH2:2]([C:5]([NH:7][C:8]1[CH:9]=[C:10]([CH:12]=[CH:13][CH:14]=1)[NH2:11])=[O:6])[CH2:3][CH3:4].[N:15]1([C:20]#[N:21])[CH2:19][CH2:18][CH2:17][CH2:16]1>ClC1C=CC=CC=1.CN(C)C1C=CN=CC=1>[ClH:1].[CH2:2]([C:5]([NH:7][C:8]1[CH:9]=[C:10]([NH:11][C:20]([N:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)=[NH:21])[CH:12]=[CH:13][CH:14]=1)=[O:6])[CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 73737Pyrrolidine-1-carbonitrileHCID 19599237N-(3-aminophenyl)butanamide hydrochloride

생성물 1

HCID 178454466HCID 178454466, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 7964Chlorobenzene용매

실험 절차

To a stirred suspension of the product of step (a), 2.3 g, 0.0135 moles, in 35ml of chlorobenzene was added 4-dimethylaminopyridine. To this was added 1-pyrrolidinecarbonitrile, 1.2 ml, 0.006 moles, and the reaction was heated to reflux for 8 hours. The reaction cooled to room temperature and the solvent was decanted. To the residue was added 25 ml of isopropanol and 150 ml of ethyl acetate. A solid crystallized and was collected by filtration. The above solid was then dried at 80° C. for 24 hours giving N-(3-(((propyl)carbonyl)amino)phenyl)-1-pyrrolidinecarboximidamide hydrochloride, 1.5 g, m.p. 207°-208° C.

후처리

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 8 hours
  3. customthe solvent was decanted
  4. additionTo the residue was added 25 ml of isopropanol and 150 ml of ethyl acetate
  5. customA solid crystallized
  6. filtrationwas collected by filtration
  7. customThe above solid was then dried at 80° C. for 24 hours

출처 및 근거

ORD 기록
ord-76ff7c163baf4af691ea5bb0c1b056d7
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05885985

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