反应详情

温度

50 °C

1.48 g (0.01 mol) of 2,2-dimethylbutyric acid chloride dissolved in 20 ml of tetrahydrofuran are added dropwise, with stirring, at ambient temperature, to a solution of 4.2 g (0.01 mol) of 5,11-dihydro-11-[[4-[3-(ethylamino)propyl]-1-piperidinyl]acetyl]-6H-pyrido-[2,3-b][1,4]benzodiazepin-6-one and 2 ml of triethylamine in 150 ml of tetrahydrofuran. In order to complete the reaction the solution is stirred for a further hour at 50° C. After cooling, the precipitated triethylamine hydrochloride is filtered off and the filtrate is evaporated to dryness using a rotary evaporator in a water jet vacuum. In order to purify it the residue is dissolved in ethyl acetate. The ethyl acetate solution is extracted twice with 10% hydrochloric acid, the organic phase is separated off and the aqueous phase is made alkaline by the addition of concentrated ammonia. Then the aqueous phase is extracted twice with ethyl acetate. The organic phase is dried over sodium sulphate and evaporated to dryness in vacuo. The residue obtained is crystallised by digesting it in ethyl acetate. Colourless crystals are obtained of m.p. 136°-138° C.

1. additionare added dropwise
2. customthe reaction the solution
3. temperatureAfter cooling
4. filtrationthe precipitated triethylamine hydrochloride is filtered off
5. customthe filtrate is evaporated to dryness
6. customa rotary evaporator in a water jet vacuum
7. customIn order to purify it the residue
8. dissolutionis dissolved in ethyl acetate
9. extractionThe ethyl acetate solution is extracted twice with 10% hydrochloric acid
10. customthe organic phase is separated off
11. additionby the addition of concentrated ammonia
12. extractionThen the aqueous phase is extracted twice with ethyl acetate
13. dry with materialThe organic phase is dried over sodium sulphate
14. customevaporated to dryness in vacuo
15. customThe residue obtained
16. customis crystallised
17. customColourless crystals are obtained of m.p. 136°-138° C.