반응 #214473

반응 방정식

4-amino-2-chloro-6,7-dimethoxyquinazoline

1-(4-piperidinyl)-pyrrolidine-2,5-dione

→

1-[1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-pyrrolidin-2,5-dione hydrochloride

용매

isoamyl alcohol

반응 조건

후처리

1. 1
   온도refluxed for 22 hours
2. 2
   온도It is cooled to 20°
3. 3
   여과filtered
4. 4
   세척the residue washed once with 250 ml of cold ethanol and twice with 250 ml of diethyl ether each
5. 5
   온도300 ml of water, the suspension heated
6. 6
   온도to reflux
7. 7
   온도immediately cooled to 20°
8. 8
   여과filtered
9. 9
   세척The residue is washed with 300 ml of cold ethanol and 200 ml of diethyl ether

실험 절차

The mixture of 215 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline, 192.3 g of 1-(4-piperidinyl)-pyrrolidine-2,5-dione and 5,600 ml of isoamyl alcohol is stirred and refluxed for 22 hours. It is cooled to 20°, filtered and the residue washed once with 250 ml of cold ethanol and twice with 250 ml of diethyl ether each. The solids are suspended in 6000 ml of ethanol and 300 ml of water, the suspension heated to reflux, immediately cooled to 20° and filtered. The residue is washed with 300 ml of cold ethanol and 200 ml of diethyl ether, to yield the 1-[1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-pyrrolidin-2,5-dione hydrochloride melting at 237° with decomposition.

출처