Hydrochloric Acid → HCID 178455691, Verbindung

HRID 591226Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 591226
[Na].[NH2:2][C:3]1[N:8]([NH2:9])[C:7](=[O:10])[CH:6]=[C:5]([CH3:11])[N:4]=1.[F:12][C:13]([F:21])([CH2:19][CH3:20])[C:14](OCC)=O.Cl>O1CCOCC1.C(O)C>[F:12][C:13]([C:14]1[N:2]=[C:3]2[N:4]=[C:5]([CH3:11])[CH:6]=[C:7]([OH:10])[N:8]2[N:9]=1)([F:21])[CH2:19][CH3:20]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 9131753-Amino-2-imino-6-methyl-2,3-dihydropyrimidin-4(1H)-oneHCID 5360545SodiumHCID 22749276Ethyl 2,2-difluorobutanoate

Produkt 1

HCID 178455691HCID 178455691, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of NaEtO prepared from sodium (FLUKA, 0.152 g, 6.62 mmol) and ethanol (25 mL), Intermediate 1 (0.773 g, 5.52 mmol) was added, and the mixture was heated at 80° C. for 30 min. Then, the reaction was cooled down to room temperature and ethyl 2,2-difluorobutanoate (FLUOROCHEM, 1007 mg, 6.62 mmol) was added and the reaction mixture was stirred at 80° C. for 3 h. A solution of HCl (1.655 mL, 6.62 mmol) in dioxane was added and a white solid was formed. The residue was purified (silica gel column, eluting with DCM:MeOH mixtures from 100:0 to 90:10%) to obtain Intermediate 6 as a white solid.

Aufarbeitung

  1. additionwas added
  2. temperatureThen, the reaction was cooled down to room temperature
  3. customa white solid was formed
  4. customThe residue was purified
  5. wash(silica gel column, eluting with DCM:MeOH mixtures from 100:0 to 90:10%)

Quellen und Nachweise

ORD-Eintrag
ord-083555a2301a4b0ab0362f0529b3cc77
Quelldatensatz
uspto-grants-2016_01
Patentnummer
US09238653B2

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