تفاعل #4270

معادلة التفاعل

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

paraformaldehyde

piperidine

→

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

المذيبات

dioxan

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةis refluxed for 1 hour
2. 2
   ترشيحare filtered off
3. 3
   أخرىthe filtrate is evaporated to dryness in vacuo
4. 4
   أخرىThe crude product is purified by column chromatography on silica gel (mobile phase: ethyl acetate, ethyl acetate+10% methanol)
5. 5
   أخرىAfter recrystallisation from ethyl acetate, 2.7 g (21% of theory) of the desired compound
6. 6
   أخرىare obtained

الإجراء التجريبي

A mixture consisting of 9.6 g (0.03 mol) of 5,11-dihydro-11-[1-oxo-4-pentynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 1.08 g (0.036 mol) of paraformaldehyde, 3.06 g (0.036 mol) of piperidine, 0.2 g of copper(I) chloride and 150 ml of dioxan is refluxed for 1 hour. After the reaction has ended the insoluble constituents are filtered off and the filtrate is evaporated to dryness in vacuo. The crude product is purified by column chromatography on silica gel (mobile phase: ethyl acetate, ethyl acetate+10% methanol). After recrystallisation from ethyl acetate, 2.7 g (21% of theory) of the desired compound are obtained, m.p. 197° C.

المصدر