Reaktionsgleichung
Cl[C:2](=[CH2:5])[C:3]#[N:4].Cl.[C:7]([CH2:10][CH2:11][CH2:12][CH2:13][N:14]1[C:18](=[O:19])[C:17]2=[CH:20][CH:21]=[CH:22][CH:23]=[C:16]2[C:15]1=[O:24])(=[NH:9])[NH2:8].N12CCCCC1C=NCCC2>C(#N)C>[NH2:4][C:3]1[CH:2]=[CH:5][N:8]=[C:7]([CH2:10][CH2:11][CH2:12][CH2:13][N:14]2[C:15](=[O:24])[C:16]3=[CH:23][CH:22]=[CH:21][CH:20]=[C:17]3[C:18]2=[O:19])[N:9]=1Komponenten
Versuchsvorschrift
A solution of 2-chloroacrylonitrile (1.75 g.) in acetronitrile (10 ml.) was added over 15 minutes to an ice-cooled mixture of 1-amidino-4-phthalimidobutane hydrochloride (5.64 g.), acetonitrile (50 ml.) and 1,5-diazabicyclo[5,4,0]undec-5-ene (6.08 g.). The mixture was stirred for a further two hours and then evaporated to dryness. The residue was treated with water (50 ml.) and the mixture extracted with ethyl acetate (2×50 ml.). The combined ethyl acetate extracts were extracted with N hydrochloric acid (3×30 ml.) and the combined aqueous extracts neutralised with sodium bicarbonate and extracted with ethyl acetate. The ethyl acetate extracts were evaporated to dryness and the residue recrystallised from acetonitrile to give 4-amino-2-(4-phthalimidobutyl)pyrimidine (2.5 g.), m.p. 139°-140°.
Aufarbeitung
- temperaturecooled
- customevaporated to dryness
- additionThe residue was treated with water (50 ml.)
- extractionthe mixture extracted with ethyl acetate (2×50 ml.)
- extractionThe combined ethyl acetate extracts were extracted with N hydrochloric acid (3×30 ml.)
- extractionextracted with ethyl acetate
- customThe ethyl acetate extracts were evaporated to dryness
- customthe residue recrystallised from acetonitrile
Quellen und Nachweise
- ORD-Eintrag
- ord-440b1d3585c8494281a1602658ea97d9
- Quelldatensatz
- uspto-grants-1988_08
- Patentnummer
- US04762932
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