Propylamine → [2-(4-Phenylpiperazin-1-yl)-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl]propylamine

HRID 1805971Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1805971
Cl[C:2]1[C:3]2[S:22][CH2:21][CH2:20][C:4]=2[N:5]=[C:6]([N:8]2[CH2:13][CH2:12][N:11]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:10][CH2:9]2)[N:7]=1.[CH2:23]([NH2:26])[CH2:24][CH3:25]>O>[C:14]1([N:11]2[CH2:12][CH2:13][N:8]([C:6]3[N:7]=[C:2]([CH2:25][CH2:24][CH2:23][NH2:26])[C:3]4[S:22][CH2:21][CH2:20][C:4]=4[N:5]=3)[CH2:9][CH2:10]2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Komponenten

4

Edukt 2

HCID 7852PropylamineHCID 866162644-Chloro-2-(4-phenylpiperazin-1-yl)-6,7-dihydrothieno[3,2-d]pyrimidine

Produkt 1

HCID 68440117[2-(4-Phenylpiperazin-1-yl)-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl]propylamineAusbeute 76 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

0.83 g (2.5 mmol) of 4-chloro-2-(4-phenylpiperazin-1-yl)-6,7-dihydrothieno[3,2-d]pyrimidine (V) is combined with 8.3 mL of n-propylamine, reacted for 0.2 hours at 130° C. in the microwave. Then the reaction mixture is added to water and extracted with dichloromethane. The organic phase is concentrated by evaporation, the residue is crystallized. The aqueous phase is extracted with ethyl acetate, the organic phase evaporated to dryness. The solids are combined and stirred with methanol. 0.68 g of the product (76%) is obtained as a powder.

Aufarbeitung

  1. customreacted for 0.2 hours at 130° C. in the microwave
  2. extractionextracted with dichloromethane
  3. concentrationThe organic phase is concentrated by evaporation
  4. customthe residue is crystallized
  5. extractionThe aqueous phase is extracted with ethyl acetate
  6. customthe organic phase evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-81fb7300023348a38472587f3d8f6f50
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08354531B2

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