Phosgene → HCID 59863032, Verbindung

HRID 2064066Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2064066
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[NH:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1.[C:23](Cl)(Cl)=[O:24].C(N(CC)CC)C>ClCCl>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:23](=[O:24])[N:9]([CH:10]3[CH2:11][CH2:12][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:14][CH2:15]3)[C:3]=2[CH:4]=1

Komponenten

5

Edukt 3

HCID 6371PhosgeneHCID 8471TriethylamineHCID 57423910HCID 57423910, Verbindung

Produkt 1

HCID 59863032HCID 59863032, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

1,1-Dimethylethyl 4-[(2-amino-5-chlorophenyl)amino]-1-piperidinecarboxylate (D28) (5.8 g) was dissolved in 100 ml of dichloromethane at 0° C. and phosgene (20% in toluene, 10 ml) and triethylamine (5.6 ml) were added and the mixture was stirred at 0° C. for 1 h, then washed with aqueous citric acid, dried over MgSO4, filtered and evaporated The product was crystallised from diethyl ether to yield the title compound, 5.7 g.

Aufarbeitung

  1. washwashed with aqueous citric acid
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. customevaporated The product
  5. customwas crystallised from diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-78cc5d8a778a4467839a0aed8a6e065e
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08288413B2

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