Ethyl 3-(2,3-dihydro-1,4-benzodioxin-6-yl)-3-oxopropanoate → HCID 178432412, Verbindung
Reaktionsgleichung
[CH3:1][C:2]1[N:3]=[C:4]([NH2:7])[NH:5][N:6]=1.[O:8]1[CH2:13][CH2:12][O:11][C:10]2[CH:14]=[C:15]([C:18](=O)[CH2:19][C:20](OCC)=[O:21])[CH:16]=[CH:17][C:9]1=2>C(O)(=O)C>[O:8]1[CH2:13][CH2:12][O:11][C:10]2[CH:14]=[C:15]([C:18]3[NH:7][C:4]4[N:5]([N:6]=[C:2]([CH3:1])[N:3]=4)[C:20](=[O:21])[CH:19]=3)[CH:16]=[CH:17][C:9]1=2Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
A mixture of 5-methyl-2H-1,2,4-triazol-3-amine (147 mg, 1.50 mmol, 1.00 equiv), acetic acid (3 mL), and ethyl 3-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-oxopropanoate (375 mg, 1.50 mmol, 1.00 equiv) was stirred for 16 hr at 120° C., then concentrated to dryness. The resulting solid was washed by 5 mL MeOH and collected by filtration. The solid was dissolved in 10 mL of NH4OH (aq.) and filtered. The filtrate was adjusted to pH<5 with HOAc, then concentrated to dryness. The resulting solid was washed by 10 mL water, collected by filtration, and dried to get 50 mg (12%) of 5-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-2-methyl-[1,2,4]triazolo[1,5-α]pyrimidin-7(4H)-one as a yellow solid.
Aufarbeitung
- concentrationconcentrated to dryness
- washThe resulting solid was washed by 5 mL MeOH
- filtrationcollected by filtration
- dissolutionThe solid was dissolved in 10 mL of NH4OH (aq.)
- filtrationfiltered
- concentrationconcentrated to dryness
- washThe resulting solid was washed by 10 mL water
- filtrationcollected by filtration
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-9832214212f84014ad6fd60a6652ddfb
- Quelldatensatz
- uspto-grants-2016_03
- Patentnummer
- US09278973B2
Notizen zur Reaktion
Wird geladen…