Reaktion #8812

Reaktionsgleichung

7-Benzyl-4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine

7-benzyl-4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine

ammonium formate

→

4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine

Ausbeute 69.3%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturto reflux for 12 h
3. 3
   SonstigeThe catalyst was removed by filtration
4. 4
   Waschenwashed with MeOH
5. 5
   Einengenthe filtrate was concentrated
6. 6
   WaschenFlash column chromatography eluting with 5% MeOH/CH2Cl2 containing 0.5% of NH4OH

Vorschrift

7-Benzyl-4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine 5a (0.55 g, 1.77 mmol) was dissolved in methanol (35 mL) under nitrogen. 10% Pd/C (0.55 g) was added under nitrogen followed by ammonium formate (1.12 g, 17.72 mmol) and the mixture was heated to reflux for 12 h. The catalyst was removed by filtration, washed with MeOH and the filtrate was concentrated. Flash column chromatography eluting with 5% MeOH/CH2Cl2 containing 0.5% of NH4OH gave 0.27 g of 4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine 6a as a pale yellow dense liquid.

Quelle