Reaktion #1989406

Reaktionsgleichung

3-aminopicolinic acid

triethylamine

methyl sarcosinate hydrochloride

→

3,4-dihydro-4-methyl-2H-pyrido[3,2-e][1,4]diazepine-2,5(1H)-dione

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo the light brown solution obtained there
2. 2
   workup.STIRRINGthe mixture is stirred at the boiling point for 6 hours
3. 3
   SonstigeAfter removing the dimethylformamide in vacuo
4. 4
   Sonstigethe residue is crystallized from ethanol

Vorschrift

A suspension of 5.18 g (37.5 mmol) of 3-aminopicolinic acid in 100 ml of dimethylformamide is treated with 6.20 g (38.2 mmol) of N,N'-carbonyldiimidazole and the mixture is stirred at room temperature for 1 hour. To the light brown solution obtained there are added 3.84 g (38 mmol) of triethylamine and 5.30 g (38 mmol) of methyl sarcosinate hydrochloride and the mixture is stirred at the boiling point for 6 hours. After removing the dimethylformamide in vacuo, the residue is crystallized from ethanol. There is obtained 3,4-dihydro-4-methyl-2H-pyrido[3,2-e][1,4]diazepine-2,5(1H)-dione of melting point 272°-274°.

Quelle