Amitrole → HCID 178515486, Verbindung

HRID 923342

Reaktionsgleichung

Reaktionsgleichung von HRID 923342
[N:1]1[NH:2][C:3]([NH2:6])=[N:4][CH:5]=1.[O:7]1[CH2:12][CH2:11][O:10][C:9]2[CH:13]=[C:14]([C:17](=O)[CH2:18][C:19](OCC)=[O:20])[CH:15]=[CH:16][C:8]1=2>C(O)(=O)C>[O:7]1[CH2:12][CH2:11][O:10][C:9]2[CH:13]=[C:14]([C:17]3[NH:6][C:3]4[N:2]([N:1]=[CH:5][N:4]=4)[C:19](=[O:20])[CH:18]=3)[CH:15]=[CH:16][C:8]1=2

Komponenten

4

Edukt 2

HCID 1639AmitroleHCID 15315318Ethyl 2,3-dihydro-β-oxo-1,4-benzodioxin-6-propanoate

Produkt 1

HCID 178515486HCID 178515486, VerbindungAusbeute 15 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 2H-1,2,4-triazol-3-amine (200 mg, 2.38 mmol, 1.00 equiv), acetic acid (3 mL), and ethyl 3-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-oxopropanoate (600 mg, 2.40 mmol, 1.01 equiv) was stirred for 24 hr at 120° C. and then concentrated to dryness. The resulting solid was washed with MeOH and collected by filtration. The solid was dissolved in 15 mL of NH4OH (aq.) and filtered. The filtrate was adjusted to pH 5 with HOAc. The resulting solid was collected by filtration and washed with water. The solid was dried to get 95 mg (15%) of 5-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-[1,2,4]triazolo[1,5-α]pyrimidin-7(4H)-one as a white solid.

Aufarbeitung

  1. concentrationconcentrated to dryness
  2. washThe resulting solid was washed with MeOH
  3. filtrationcollected by filtration
  4. dissolutionThe solid was dissolved in 15 mL of NH4OH (aq.)
  5. filtrationfiltered
  6. filtrationThe resulting solid was collected by filtration
  7. washwashed with water
  8. customThe solid was dried

Quellen und Nachweise

ORD-Eintrag
ord-bde312b457114b68bc8a3ac5eae6bfc4
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09278973B2

Verknüpfte Notizen

Wird geladen…