Formamide → 1,5,6,7-Tetrahydro-4H-cyclopenta(4,5)thieno(2,3-d)pyrimidin-4-one
Reaktionsgleichung
[NH2:1][C:2]1[S:6][C:5]2[CH2:7][CH2:8][CH2:9][C:4]=2[C:3]=1[C:10]([O:12]CC)=O.O.[CH:16]([NH2:18])=O>>[N:1]1[C:2]2[S:6][C:5]3[CH2:7][CH2:8][CH2:9][C:4]=3[C:3]=2[C:10](=[O:12])[NH:18][CH:16]=1Komponenten
4
Versuchsvorschrift
A suspension of 11.37 g ethyl 2-amino-5,6-dihydro-4H-cyclopenta[b]thiophene-3-carboxylate in 40 mL formamide was heated for 4 h to 190° C. using a heating mantle, then cooled and poured into 400 mL water. The mixture was then filtered to remove the solid product. The solids were washed successively with 30 mL EtOAc and 200 mL diethyl ether, air dried overnight, then vacuum oven dried for 3 h. The material was used in the subsequent reactions without further purification.
Aufarbeitung
- temperaturewas heated for 4 h to 190° C.
- temperaturecooled
- filtrationThe mixture was then filtered
- customto remove the solid product
- washThe solids were washed successively with 30 mL EtOAc and 200 mL diethyl ether, air
- customdried overnight
- customvacuum oven dried for 3 h
- customThe material was used in the subsequent reactions without further purification
Quellen und Nachweise
- ORD-Eintrag
- ord-7015bc9ba75548c697063adb8e79b4d9
- Quelldatensatz
- uspto-grants-2005_02
- Patentnummer
- US06849638B2
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