1,2-Dichloroethane → HCID 178452376, Verbindung

HRID 1185593Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1185593
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([C:12]([OH:14])=O)[CH:3]=1.[CH2:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][N:25]([C:28](=[O:31])[CH2:29][NH2:30])[CH2:24][CH2:23]1)=[O:21])[CH2:16][CH2:17][CH3:18].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C=O)C.O>[CH2:15]([O:19][C:20]([N:22]1[CH2:23][CH2:24][N:25]([C:28](=[O:31])[CH2:29][NH:30][C:12]([C:4]2[CH:3]=[C:2]([OH:1])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[N:5]=2)=[O:14])[CH2:26][CH2:27]1)=[O:21])[CH2:16][CH2:17][CH3:18]

Komponenten

7

Edukt 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 667130634-(2-Amino-acetyl)-piperazine-1-carboxylic acid butyl esterHCID 178418933HCID 178418933, Verbindung

Produkt 1

HCID 178452376HCID 178452376, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 9.5 g of 4-Hydroxy-quinoline-2-carboxylic acid and 12.2 g of 4-(2-Amino-acetyl)-piperazine-1-carboxylic acid butyl ester in 110 ml of DMF, 7.7 g of HOBT and 9.6 g of EDC was added and the reaction mixture was stirred for 16 h at RT. Then, the reaction mixture was diluted with water and extracted with DCM. The combined organic phases were dried over MgSO4 and the solvents were removed under reduced pressure. The isolated crude product was used in the next reaction step. Yield: 23 g.

Aufarbeitung

  1. extractionextracted with DCM
  2. dry with materialThe combined organic phases were dried over MgSO4
  3. customthe solvents were removed under reduced pressure
  4. customThe isolated crude product
  5. customwas used in the next reaction step

Quellen und Nachweise

ORD-Eintrag
ord-1ee5a3baee454be6a10eccbbf6eade0e
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08669266B2

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