2-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol monophosphate → 2-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol

HRID 71215

Reaktionsgleichung

Reaktionsgleichung von HRID 71215
P([O:5][C:6]([C@@:9]1([O:32][C:33]2[CH:38]=[C:37]([F:39])[C:36]([F:40])=[C:35]([F:41])[CH:34]=2)[CH2:14][CH2:13][CH2:12][N:11]2[C:15]([C:18]3[CH:23]=[CH:22][C:21]([N:24]4[CH:28]=[C:27]([CH3:29])[N:26]=[CH:25]4)=[C:20]([O:30][CH3:31])[N:19]=3)=[N:16][N:17]=[C:10]12)([CH3:8])[CH3:7])(O)(O)=O>C(O)C>[CH3:31][O:30][C:20]1[N:19]=[C:18]([C:15]2[N:11]3[CH2:12][CH2:13][CH2:14][C@@:9]([C:6]([OH:5])([CH3:8])[CH3:7])([O:32][C:33]4[CH:38]=[C:37]([F:39])[C:36]([F:40])=[C:35]([F:41])[CH:34]=4)[C:10]3=[N:17][N:16]=2)[CH:23]=[CH:22][C:21]=1[N:24]1[CH:28]=[C:27]([CH3:29])[N:26]=[CH:25]1

Komponenten

3

Edukt 1

HCID 666076052-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol monophosphate

Produkt 1

HCID 569296452-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-olAusbeute 99,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To 2-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol monophosphate (213.4 g) was added ethanol (350 mL), the mixture was dissolved at 60° C., and the insoluble material was removed by filtration. 2-Propanol (700 mL) was added to the filtrate at 60° C., and the mixture was stirred for 30 min, and at 0° C. for 30 min. The crystals were collected by filtration, washed with 2-propanol (250 mL) and dried at 60° C. under reduced pressure to give the title compound (184 g).

Aufarbeitung

  1. dissolutionthe mixture was dissolved at 60° C.
  2. customthe insoluble material was removed by filtration
  3. addition2-Propanol (700 mL) was added to the filtrate at 60° C.
  4. waitat 0° C. for 30 min
  5. filtrationThe crystals were collected by filtration
  6. washwashed with 2-propanol (250 mL)
  7. customdried at 60° C. under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6de4c89218ca4b7295f0f7a3ecdbc037
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822699B2

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