反応 #214473

反応方程式

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

溶媒

isoamyl alcohol

反応条件

後処理

1. 1
   温度refluxed for 22 hours
2. 2
   温度It is cooled to 20°
3. 3
   ろ過filtered
4. 4
   洗浄the residue washed once with 250 ml of cold ethanol and twice with 250 ml of diethyl ether each
5. 5
   温度300 ml of water, the suspension heated
6. 6
   温度to reflux
7. 7
   温度immediately cooled to 20°
8. 8
   ろ過filtered
9. 9
   洗浄The residue is washed with 300 ml of cold ethanol and 200 ml of diethyl ether

実験手順

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.

出典