Methanol → 7-Chloro-5-[(2,3-difluorophenylmethyl)thio]-2-methoxythiazolo[4,5-d]pyrimidine

HRID 1097361Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1097361
Br[C:2]1[S:3][C:4]2[C:9]([Cl:10])=[N:8][C:7]([S:11][CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[C:14]=3[F:20])=[N:6][C:5]=2[N:21]=1.[OH-:22].[K+].[CH3:24]O>Cl>[Cl:10][C:9]1[C:4]2[S:3][C:2]([O:22][CH3:24])=[N:21][C:5]=2[N:6]=[C:7]([S:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[C:14]=2[F:20])[N:8]=1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 226713342-Bromo-7-chloro-5-((2,3-difluorobenzyl)thio)thiazolo[4,5-d]pyrimidine

Produkt 1

HCID 226713137-Chloro-5-[(2,3-difluorophenylmethyl)thio]-2-methoxythiazolo[4,5-d]pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidKatalysator

Versuchsvorschrift

The product of example 31 step a) (5.6 g) was suspended in methanol (150 ml) and potassium hydroxide powder (0.77 g) added. The whole was stirred at room temperature for 2 hours. The mixture was adjusted to pH 7 with a few drops of concentrated hydrochloric acid before it was evaporated to dryness. Purified by column chromatography (silica—3:2 to 1:1 isohexane/dichloromethane) to give white solid (2.0 g).

Aufarbeitung

  1. customwas evaporated to dryness
  2. customPurified by column chromatography (silica—3:2 to 1:1 isohexane/dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-74c6680aa43d45aeb301dda4bd5924aa
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08143261B2

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