Potassium Carbonate → HCID 14074168, Verbindung

HRID 620042

Reaktionsgleichung

Reaktionsgleichung von HRID 620042
Br.Br.[OH:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1.Cl[C:17]1[O:18][C:19]2[CH:25]=[CH:24][CH:23]=[CH:22][C:20]=2[N:21]=1.C([O-])([O-])=O.[K+].[K+]>CN(C)C=O>[OH:3][C:4]1[CH:5]=[CH:6][C:7]([N:10]2[CH2:15][CH2:14][N:13]([C:17]3[O:18][C:19]4[CH:25]=[CH:24][CH:23]=[CH:22][C:20]=4[N:21]=3)[CH2:12][CH2:11]2)=[CH:8][CH:9]=1

Komponenten

5

Edukt 3

HCID 11430Potassium Carbonate3×HCID 119862-ChlorobenzoxazoleHCID 2723591p-(1-Piperazinyl)phenol dihydrobromide

Produkt 1

HCID 14074168HCID 14074168, VerbindungAusbeute 97,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

A mixture of 5.11 g (15 mmol) of 1-(4-hydroxyphenyl)piperazine dihydrobromide, 2.46 g (16 mmol) of 2-chlorobenzoxazole and 2.18 g (15.8 mmol) of powdered K2CO3 in 55 ml of absolute N,N-dimethylformamide was warmed to 85° C., and 345 mg of powdered K2CO3 were added with stirring under a nitrogen atmosphere in each case after 10 minutes, after a further 25 minutes and after a further 60 minutes (total addition of 1.035 g (7.5 mmol) of K2CO3). The mixture was stirred for a further 3 hours at 85° C., the DMF was substantially removed by distillation in an oil-pump vacuum in a rotary evaporator, the crystalline residue was mixed with 50 ml of water, and this mixture was shaken for 15 minutes. The mixture was then filtered under suction and the filter residue was washed with water and dried in vacuo. 4.30 g (97% of theory) of pure 1-(4-hydroxyphenyl)-4-(benzoxazol-2-yl)piperazine, melting point 161°-3° C., were obtained,

Aufarbeitung

  1. stirringThe mixture was stirred for a further 3 hours at 85° C.
  2. customthe DMF was substantially removed by distillation in an oil-pump vacuum in a rotary evaporator
  3. additionthe crystalline residue was mixed with 50 ml of water
  4. stirringthis mixture was shaken for 15 minutes
  5. filtrationThe mixture was then filtered under suction
  6. washthe filter residue was washed with water
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3f4b8fdb47f94dfdab03d170978fb3fe
Quelldatensatz
uspto-grants-1989_04
Patentnummer
US04818758

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