Water → Dimethyl[[6-(2-methylpropionamido)-4-quinazolinylamino]methylene]propanedioate

HRID 354886

Reaktionsgleichung

Reaktionsgleichung von HRID 354886
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([NH:12][C:13](=[O:17])[CH:14]([CH3:16])[CH3:15])[CH:10]=2)[N:5]=[CH:4][N:3]=1.CO[CH:20]=[C:21]([C:26]([O:28][CH3:29])=[O:27])[C:22]([O:24][CH3:25])=[O:23].O>CN(C)C=O>[CH3:16][CH:14]([CH3:15])[C:13]([NH:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[N:5]=[CH:4][N:3]=[C:2]2[NH:1][CH:20]=[C:21]([C:26]([O:28][CH3:29])=[O:27])[C:22]([O:24][CH3:25])=[O:23])=[O:17]

Komponenten

5

Edukt 3

HCID 962WaterHCID 90770Dimethyl methoxymethylenemalonateHCID 130604634-Amino-6-(2-methylpropionamido)quinazoline

Produkt 1

HCID 13302083Dimethyl[[6-(2-methylpropionamido)-4-quinazolinylamino]methylene]propanedioateAusbeute 88,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 4-amino-6-(2-methylpropionamido)quinazoline (6.2 g) and dimethyl methoxymethylenepropanedioate (7.01 g) in N,N-dimethylformamide (25 ml) was stirred at 100° C. for 1.5 hours and cooled to room temperature. Water was added to the reaction mixture. The resulting solid was separated by filtration, washed with water and dried to give dimethyl [[6-(2-methylpropionamido)-4-quinazolinylamino]methylene]propanedioate (8.9 g). Recrystallization from ethyl acetate gave pure crystals melting at 212°-214° C.

Aufarbeitung

  1. temperaturecooled to room temperature
  2. customThe resulting solid was separated by filtration
  3. washwashed with water
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-cad331055bdc4453a6d68fc626ac5988
Quelldatensatz
uspto-grants-1983_03
Patentnummer
US04377580

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