Ammonia → HCID 58709443, Verbindung

HRID 18675Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 18675
[NH3:1].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:14](=[O:15])[CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[N:11]([CH3:20])[C:10]2=[O:21])=[CH:5][C:4]=1[S:22](Cl)(=[O:24])=[O:23].C(OCC)(=O)C.Cl>O1CCCC1>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:14](=[O:15])[CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[N:11]([CH3:20])[C:10]2=[O:21])=[CH:5][C:4]=1[S:22]([NH2:1])(=[O:24])=[O:23]

Komponenten

6

Edukt 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 153348022-chloro-5-(3,6-dihydro-3-methyl-4-trifluoromethyl-2,6-dioxo-1(2H)pyrimidinyl)benzenesulfonyl chloride

Produkt 1

HCID 58709443HCID 58709443, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

With stirring, 1.6 g (93.8 mmol) of ammonia gas were, at 0° C., introduced into a mixture of 18 g (44.6 mmol) of 2-chloro-5-[3,6-dihydro-3-methyl-2,6-dioxo-4-trifluoromethyl-(2H)-pyrimidin-1-yl]-benzenesulfonylchloride in tetrahydrofuran (THF). Then, at 10° C., ethyl acetate was added and the mixture was acidified with 1N hydrochloric acid. The phases were separated and the aqueous phase was extracted, and the combined organic phases were then washed, dried and the solvent was removed. Customary purification methods gave 14.4 g (82.4% of theory) of the title compound (m.p.: 257-258° C.).

Aufarbeitung

  1. customwere, at 0° C.
  2. customThe phases were separated
  3. extractionthe aqueous phase was extracted
  4. washthe combined organic phases were then washed
  5. customdried
  6. customthe solvent was removed
  7. customCustomary purification methods

Quellen und Nachweise

ORD-Eintrag
ord-767ea4798cf34ce680042a650d7279d7
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07741485B2

Notizen zur Reaktion

Wird geladen…