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Pyrrolidine-1-carbonitrile → HCID 178479317, 화합물

HRID 1418846
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HRID 1418846 반응식
[ClH:1].[C:2]1([CH2:8][CH2:9][C:10]([NH:12][C:13]2[CH:14]=[C:15]([CH:17]=[CH:18][CH:19]=2)[NH2:16])=[O:11])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:20]1([C:25]#[N:26])[CH2:24][CH2:23][CH2:22][CH2:21]1>ClC1C=CC=CC=1.CN(C)C1C=CN=CC=1>[ClH:1].[C:2]1([CH2:8][CH2:9][C:10]([NH:12][C:13]2[CH:14]=[C:15]([NH:16][C:25]([N:20]3[CH2:24][CH2:23][CH2:22][CH2:21]3)=[NH:26])[CH:17]=[CH:18][CH:19]=2)=[O:11])[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 73737Pyrrolidine-1-carbonitrileHCID 195992863-(((2-Phenylethyl)carbonyl)amino)aniline hydrochloride

생성물 1

HCID 178479317HCID 178479317, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 7964Chlorobenzene용매

실험 절차

To a stirred suspension of the product of step (a), 2.0 g, 0.006 moles, in 35 ml of chlorobenzene was added 4-dimethylaminopyridine. To this was added 1-pyrrolidinecarbonitrile, 1.2 ml, 0.06 moles, and the reaction was heated to reflux for 4 hours. The reaction was cooled to room temperature and the solvent 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 60° C. for 24 hours giving 700 mg of N-(3-(((2-phenylethyl)carbonyl)amino)phenyl)-1-pyrrolidinecarboximidamide hydrochloride, m.p. 220°-221° C.

후처리

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 4 hours
  3. customthe solvent 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 60° C. for 24 hours

출처 및 근거

ORD 기록
ord-c42bade2c6de45c29689202e22862336
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05885985

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