Diisopropylethylamine → HCID 10110753, Verbindung

HRID 860177Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 860177
[CH2:1]([O:8][C:9](=[O:20])[CH:10]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:11]([OH:13])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[C:22]([C:25]1[CH:31]=[CH:30][C:28]([NH2:29])=[CH:27][CH:26]=1)(=[NH:24])[NH2:23].[B-](F)(F)(F)F.CCOC(C(C#N)=NOC(N(C)C)=[N+](C)C)=O.CCN(C(C)C)C(C)C>CN(C=O)C>[CH2:1]([O:8][C:9](=[O:20])[CH:10]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:11]([NH:29][C:28]1[CH:30]=[CH:31][C:25]([C:22](=[NH:23])[NH2:24])=[CH:26][CH:27]=1)=[O:13])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

6

Edukt 4

HCID 81531DiisopropylethylamineHCID 117278Propanedioic acid, 2-phenyl-, 1-(phenylmethyl) esterHCID 122765Benzenecarboximidamide, 4-amino-, hydrochloride (1:1)HCID 2733286O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborate

Produkt 1

HCID 10110753HCID 10110753, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

10 g (37 mmol) phenyl malonic acid monobenzyl ester and 7.7 g (37 mmol) 4-amidino aniline hydrochloride were dissolved in 60 ml DMF and cooled to 0° C. 12.2 g (37 mmol) TOTU and 19 ml (111 mmol) DIPEA were added and the mixture stirred at rt overnight. The solvent was removed, the residue taken up in ethyl acetate, and extracted with 10% sodium carbonate solution and brine. After drying over sodium sulfate, the solution was evaporated to dryness and extracted with diethyl ether twice. The remaining solid product was sufficiently pure.

Aufarbeitung

  1. customThe solvent was removed
  2. extractionextracted with 10% sodium carbonate solution and brine
  3. dry with materialAfter drying over sodium sulfate
  4. customthe solution was evaporated to dryness
  5. extractionextracted with diethyl ether twice

Quellen und Nachweise

ORD-Eintrag
ord-c428ea3bc47b4a69b4669247d5a38618
Quelldatensatz
uspto-grants-2006_12
Patentnummer
US07153876B2

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