1-Methylpiperazine → HCID 20554355, Verbindung

HRID 1106027Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1106027
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.Cl[CH2:9][C:10]([N:12]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[N:16]([CH3:23])[C:15](=[O:24])[C:14]2[CH:25]=[N:26][CH:27]=[N:28][C:13]1=2)=[O:11].C(=O)(O)[O-].[Na+]>C1C=CC=CC=1>[CH3:23][N:16]1[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[N:12]([C:10](=[O:11])[CH2:9][N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)[C:13]2[N:28]=[CH:27][N:26]=[CH:25][C:14]=2[C:15]1=[O:24]

Komponenten

5

Edukt 3

HCID 531671-MethylpiperazineHCID 516892Sodium BicarbonateHCID 20554401HCID 20554401, Verbindung

Produkt 1

HCID 20554355HCID 20554355, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

2.6 g (0.0266 mol) of N-methylpiperazine are added dropwise at 50° C., in the course of 15 minutes, to a suspension of 4.0 g (0.0133 mol) of 11-chloroacetyl-6-methyl-5,6-dihydropyrimido[4,5-b][1,5]benzodiazepin-5-one in 30 ml of absolute benzene, and the mixture is stirred for a further 1.5 hours at 70° C. After cooling, the mixture is poured into 100 ml of saturated sodium bicarbonate solution and is extracted once with 50 ml of ethyl acetate and twice with 100 ml, each time, of chloroform. After drying, the organic phase is concentrated in vacuo, and the liquid residue is induced to crystallize by means of ether. It is purified by filtering through neutral silica gel (elution with chloroform) and evaporating the filtrate; yield: 2.7 g, m.p. 183° to 185° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionis extracted once with 50 ml of ethyl acetate and twice with 100 ml
  3. customAfter drying
  4. concentrationthe organic phase is concentrated in vacuo
  5. customto crystallize by means of ether
  6. customIt is purified
  7. filtrationby filtering through neutral silica gel (elution with chloroform)
  8. customevaporating the filtrate

Quellen und Nachweise

ORD-Eintrag
ord-6898a588d5d343bbb43b4a8e2a4951ab
Quelldatensatz
uspto-grants-1982_01
Patentnummer
US04311700

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