Hydrochloric Acid → 5-Bromo-n4-isopropyl-n2-(4-methylsulphanylphenyl)pyrimidine-2,4-diamine

HRID 548947

Reaktionsgleichung

Reaktionsgleichung von HRID 548947
CC1C=C[C:5]([S:8]([N-]Cl)(=O)=O)=CC=1.O.O.O.[Na+].Cl.[Br:18][C:19]1[C:20]([NH:34][CH:35]([CH3:37])[CH3:36])=[N:21][C:22]([NH:25][C:26]2[CH:31]=[CH:30][C:29](C)=[CH:28][C:27]=2S)=[N:23][CH:24]=1>C(#N)C.C(OCC)(=O)C>[Br:18][C:19]1[C:20]([NH:34][CH:35]([CH3:37])[CH3:36])=[N:21][C:22]([NH:25][C:26]2[CH:31]=[CH:30][C:29]([S:8][CH3:5])=[CH:28][CH:27]=2)=[N:23][CH:24]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 517414chloramine-T trihydrateHCID 1317288425-Bromo-n4-isopropyl-n2-(4-methyl-sulphanylphenyl)pyrimidine-2,4-diamine

Produkt 1

HCID 596740705-Bromo-n4-isopropyl-n2-(4-methylsulphanylphenyl)pyrimidine-2,4-diamine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

1.36 g (4.8 mmol) of chloramine-T trihydrate (Aldrich) are added to a suspension of 1.56 g (4.0 mmol) of the hydrochloride of 5-bromo-N4-isopropyl-N2-(4-methyl-sulphanylphenyl)pyrimidine-2,4-diamine in 20 ml of acetonitrile at room temperature. The mixture is stirred at room temperature for 16 hours and then diluted with ethyl acetate. The mixture is filtered with suction and the filter cake is washed with ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated. The resulting residue is purified by HPLC:

Aufarbeitung

  1. filtrationThe mixture is filtered with suction
  2. washthe filter cake is washed with ethyl acetate
  3. dry with materialThe combined organic phases are dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe resulting residue is purified by HPLC

Quellen und Nachweise

ORD-Eintrag
ord-038419359e4a4eff90deb757ec39e87f
Quelldatensatz
uspto-grants-2011_05
Patentnummer
US07943629B2

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