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Dicyclohexylcarbodiimide → HCID 178512296, 화합물

HRID 864486
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HRID 864486 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 178512296HCID 178512296, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-2f5c64496bf24f46bd86a4b03a980dc2
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05563160

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