Acetone → HCID 131719041, Verbindung

HRID 1647764Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1647764
[CH3:1][CH:2]([CH3:35])[CH2:3][O:4][C:5](=[O:34])[CH2:6][NH:7][C:8](=[O:33])[C@H:9]([CH2:17][N:18]1[CH2:23][CH2:22][C@:21]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([OH:31])[CH:26]=2)([CH3:24])[C@@H:20]([CH3:32])[CH2:19]1)[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[C:36]([OH:44])(=[O:43])[C@H:37]([CH2:39][C:40]([OH:42])=[O:41])[OH:38].[CH3:45]C(C)=O>C(OCC)(=O)C>[C:36]([OH:44])(=[O:43])[CH:37]([CH2:39][C:40]([OH:42])=[O:41])[OH:38].[CH3:45][CH:3]([O:4][C:5](=[O:34])[CH2:6][NH:7][C:8](=[O:33])[C@H:9]([CH2:17][N:18]1[CH2:23][CH2:22][C@:21]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([OH:31])[CH:26]=2)([CH3:24])[C@@H:20]([CH3:32])[CH2:19]1)[CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)[CH2:2][CH3:1].[C:36]([OH:44])(=[O:43])[CH:37]([CH2:39][C:40]([OH:42])=[O:41])[OH:38].[C:36]([OH:44])(=[O:43])[CH:37]([CH2:39][C:40]([OH:42])=[O:41])[OH:38].[OH:31][C:27]1[CH:26]=[C:25]([C@:21]2([CH3:24])[CH2:22][CH2:23][N:18]([CH2:17][C@H:9]([CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:8]([NH:7][CH2:6][C:5]([O:4][CH:3]([CH3:36])[CH2:2][CH3:35])=[O:34])=[O:33])[CH2:19][C@@H:20]2[CH3:32])[CH:30]=[CH:29][CH:28]=1

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 222656L-Malic Acid2×HCID 9871231HCID 9871231, Verbindung

Produkt 1

HCID 131719041HCID 131719041, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A compound of Example 1, (2.5 g, 5.2 mmol, 1.0 equiv) was dissolved in 50 mL of ethyl acetate. L-malic acid (1.03 g, 7.8 mmol, 1.5 eq) was added to the mixture. After the L-malic acid was dissolved by stirring, the solution was heated to 70° C. and 4.0 mL of acetone was added. The solution was crystallized. The product was isolated by filtration. The filter cake was washed with ethyl acetate. The salt was dried until the ethyl acetate levels were below 1%. The title compound was isolated as a white crystal. The sample was analyzed using x-ray powder diffraction. mp 94°-950C.

Aufarbeitung

  1. customThe solution was crystallized
  2. customThe product was isolated by filtration
  3. washThe filter cake was washed with ethyl acetate
  4. dry with materialThe salt was dried until the ethyl acetate levels

Quellen und Nachweise

ORD-Eintrag
ord-18b0787fd8154d95a574992f90ab913a
Quelldatensatz
uspto-grants-1995_07
Patentnummer
US05434171

Notizen zur Reaktion

Wird geladen…