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Dicyclohexylcarbodiimide → HCID 178512296、化合物

HRID 864486
ノート
印刷プレビュー

反応式

HRID 864486 の反応式
[C:1]([NH:3][C:4]([NH:6][C:7]1[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=1)=S)#[N:2].[C:13]1([NH:19][CH2:20][CH2:21][NH2:22])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C=O>[C:1]([NH:3][C:4]([NH:22][CH2:21][CH2:20][NH:19][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[N:6][C:7]1[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=1)#[N:2]
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 3

HCID 10868DicyclohexylcarbodiimideHCID 742701,2-Ethanediamine, N1-phenyl-HCID 13358277N-Cyano-N'-pyridin-4-ylthiourea

生成物 1

HCID 178512296HCID 178512296、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-Cyano-N'-4-pyridylthiourea (1.80 g) was suspended in dimethylformamide (5 ml). While stirring in an ice bath N-phenylethylenediamine (1.4 ml) and N,N'-dicyclohexylcarbodiimide (2.50 g) were added, resulting in a clear solution. The mixture was left at room temperature for 3 days, when the suspension formed was evaporated extensively under high vacuum. The residue was triturated repeatedly with ether (15 ml portions), and the residual solid was extracted with 1N hydrochloric acid (50 ml). After filtration, the crude product was precipitated from the filtrate by addition of 9N sodium hydroxide and taken up into ethyl acetate (3×75 ml).

後処理

  1. additionwere added
  2. customresulting in a clear solution
  3. customwhen the suspension formed
  4. customwas evaporated extensively under high vacuum
  5. customThe residue was triturated repeatedly with ether (15 ml portions)
  6. extractionthe residual solid was extracted with 1N hydrochloric acid (50 ml)
  7. filtrationAfter filtration
  8. customthe crude product was precipitated from the filtrate by addition of 9N sodium hydroxide

出典と根拠

ORDレコード
ord-2f5c64496bf24f46bd86a4b03a980dc2
出典データセット
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05563160

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート