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Pyrrolidine-1-carbonitrile → HCID 178479312、化合物

HRID 609565
ノート
印刷プレビュー

反応式

HRID 609565 の反応式
[ClH:1].[C:2]1([CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]([C:15]2[CH:16]=[C:17]([CH:19]=[CH:20][CH:21]=2)[NH2:18])=[O:14])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:22]1([C:27]#[N:28])[CH2:26][CH2:25][CH2:24][CH2:23]1>ClC1C=CC=CC=1.CN(C)C1C=CN=CC=1>[ClH:1].[C:2]1([CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]([C:15]2[CH:16]=[C:17]([NH:18][C:27]([N:22]3[CH2:26][CH2:25][CH2:24][CH2:23]3)=[NH:28])[CH:19]=[CH:20][CH:21]=2)=[O:14])[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 73737Pyrrolidine-1-carbonitrileHCID 193536943-(((4-Phenylbutyl)amino)carbonyl)aniline hydrochloride

生成物 1

HCID 178479312HCID 178479312、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 7964Chlorobenzene溶媒

実験手順

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, 1.5 ml; 0.008 moles, and the reaction was heated to reflux for 4 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 to give N-[3-(((4-phenylbutyl)amino)carbonyl)phenyl]-1-pyrrolidinecarboximidamide hydrochloride, 2.3 g, m.p. 197-198° C.

後処理

  1. temperature0.008 moles, and the reaction was heated
  2. temperatureto reflux for 4 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

出典と根拠

ORDレコード
ord-6497bc1083d54343bd4263b16d49df8a
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998399

反応ノート

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