D-Tartaric acid → (5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol D-Tartrate

HRID 218356Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 218356
[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[N:9]=[C:10]([N:28]2[CH2:33][CH2:32][O:31][CH2:30][C@@H:29]2[CH3:34])[C:11]2[CH:17]=[CH:16][C:15]([C:18]3[CH:19]=[CH:20][C:21]([O:26][CH3:27])=[C:22]([CH2:24][OH:25])[CH:23]=3)=[N:14][C:12]=2[N:13]=1.[C:35]([OH:44])(=[O:43])[C@H:36]([C@@H:38]([C:40]([OH:42])=[O:41])[OH:39])[OH:37]>>[C:40]([C@H:38]([C@@H:36]([C:35]([OH:44])=[O:43])[OH:37])[OH:39])([OH:42])=[O:41].[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[N:9]=[C:10]([N:28]2[CH2:33][CH2:32][O:31][CH2:30][C@@H:29]2[CH3:34])[C:11]2[CH:17]=[CH:16][C:15]([C:18]3[CH:19]=[CH:20][C:21]([O:26][CH3:27])=[C:22]([CH2:24][OH:25])[CH:23]=3)=[N:14][C:12]=2[N:13]=1

Komponenten

3

Edukt 2

HCID 439655D-Tartaric acidHCID 25262965Azd8055

Produkt 1

HCID 69031901(5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol D-Tartrate

Versuchsvorschrift

(5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol (1.50 g (96% w/w, 3.1 mmoles), D-tartaric Acid (0.51 g, 3.4 mmoles) and methylated spirit industrial 74 O.P. (15.0 ml) were charged to a 100 ml reactor and heated to reflux. Product began to precipitate. On cooling more product precipitated. Product was isolated, washed with methylated spirit industrial 74 O.P. and dried in vacuum oven at 50 C for 4 h to yield 1.98 g of (5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol D-Tartrate as a yellow solid.

Aufarbeitung

  1. addition(15.0 ml) were charged to a 100 ml reactor
  2. temperatureheated to reflux
  3. customto precipitate
  4. temperatureOn cooling more product
  5. customprecipitated
  6. customProduct was isolated
  7. washwashed with methylated spirit industrial 74 O.P
  8. customand dried in vacuum oven at 50 C for 4 h

Quellen und Nachweise

ORD-Eintrag
ord-4e1ed4ceb435415093405d316ac36221
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08198441B2

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