反応 #4271

反応方程式

5,11-dihydro-11-[1-oxo-2-methyl-4-pentynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

N-methylpiperazine

maleic acid

paraformaldehyde

→

5,11-Dihydro-11-[1-oxo-2-methyl-6-(4-methyl-1-piperazinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

溶媒

water

dioxan

反応条件

後処理

1. 1
   温度is refluxed for 2 hours
2. 2
   ろ過is filtered over activated charcoal
3. 3
   その他to remove the insoluble components
4. 4
   その他the filtrate is evaporated to dryness in vacuo
5. 5
   その他In order to purify it
6. 6
   ろ過The insoluble matter is filtered off
7. 7
   workup.ADDITIONby the addition of potassium carbonate
8. 8
   その他the resin precipitated
9. 9
   乾燥After drying over magnesium sulphate
10. 10
    その他the solution is evaporated to dryness in vacuo
11. 11
    ろ過filtered
12. 12
    温度after cooling
13. 13
    その他is obtained which melts at 212° to 214° C.
14. 14
    洗浄after washing with ether

実験手順

A reaction mixture consisting of 36.6 g (0.12 mol) of 5,11-dihydro-11-[1-oxo-2-methyl-4-pentynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 4 g (0.13 mol) of paraformaldehyde, 13.2 g (0.13 mol) of N-methylpiperazine, 0.2 g of copper(I) chloride and 600 ml of dioxan is refluxed for 2 hours. After the reaction has ended the mixture is filtered over activated charcoal to remove the insoluble components and the filtrate is evaporated to dryness in vacuo. In order to purify it, the crude product is suspended in a solution of 15.4 g (0.13 mol) of maleic acid in 600 ml of water and stirred for 1 hour at ambient temperature. The insoluble matter is filtered off, the filtrate is made alkaline by the addition of potassium carbonate and the resin precipitated is taken up in 600 ml of methylene chloride. After drying over magnesium sulphate, the solution is evaporated to dryness in vacuo. The crystalline residue is decocted with 150 ml of ethyl acetate and suction filtered after cooling. By digesting it in a little ethyl acetate a crystalline product is obtained which melts at 212° to 214° C. after washing with ether.

出典