Saccharin → 4-(Dimethylamino)butyl 2-(4-((2-amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)methyl)phenyl)acetate disaccharin salt

HRID 445050Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 445050
[S:1]1([C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:5](=[O:6])[NH:4]1)(=[O:3])=[O:2].[NH2:13][C:14]1[N:19]=[C:18]([CH3:20])[C:17]([CH2:21][C:22]2[CH:27]=[CH:26][C:25]([CH2:28][C:29]([O:31][CH2:32][CH2:33][CH2:34][CH2:35][N:36]([CH3:38])[CH3:37])=[O:30])=[CH:24][CH:23]=2)=[C:16]([NH:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[N:15]=1>C(#N)C.CCOC(C)=O>[S:1]1([C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:5](=[O:6])[NH:4]1)(=[O:2])=[O:3].[S:1]1([C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:5](=[O:6])[NH:4]1)(=[O:2])=[O:3].[NH2:13][C:14]1[N:19]=[C:18]([CH3:20])[C:17]([CH2:21][C:22]2[CH:23]=[CH:24][C:25]([CH2:28][C:29]([O:31][CH2:32][CH2:33][CH2:34][CH2:35][N:36]([CH3:37])[CH3:38])=[O:30])=[CH:26][CH:27]=2)=[C:16]([NH:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[N:15]=1

Komponenten

5

Edukt 2

HCID 5143SaccharinHCID 497799954-(Dimethylamino)butyl 2-[4-[[2-amino-4-methyl-6-(pentylamino)pyrimidin-5-yl]methyl]phenyl]acetate

Produkt 1

HCID 497799944-(Dimethylamino)butyl 2-(4-((2-amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)methyl)phenyl)acetate disaccharin salt

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

Saccharin (41.5 g) was added to a stirred solution of the product from step (vi) (50.0 g) in acetonitrile (150 mL). The mixture was heated to 40° C. and stirred at the temperature for 10 minutes. The mixture was diluted with EtOAc (500 mL), seeded with Form A crystals and stirred at 40° C. for 5 hours. The mixture was then cooled to 20° C. and stirred at the temperature for 2 hours. The resulting solid was collected by filtration, washed with EtOAc (200 mL) and dried under reduced pressure to give a crude sample of the subtitle compound as a white solid, 81.5 g.

Aufarbeitung

  1. stirringstirred at 40° C. for 5 hours
  2. temperatureThe mixture was then cooled to 20° C.
  3. stirringstirred at the temperature for 2 hours
  4. filtrationThe resulting solid was collected by filtration
  5. washwashed with EtOAc (200 mL)
  6. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-db2f0160f2904fe39fafac1482ba442b
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08476288B2

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