反应详情

温度

50 °C

1.65 G. of sodium in 60 ml. of absolute ethanol are treated dropwise with 11.4 g. of dibenzo[b,e]thiepin-11(6H)-one-oxime in 60 ml. of absolute ethanol. The mixture is stirred at 50° C. for 3 hours and then cooled to 5°-10° C. The mixture is then treated dropwise with 15.3 g. of 3-diethylamino-propyl chloride, stirred at 50° C. for 16 hours and subsequently evaporated under reduced pressure. The residue is dissolved in chloroform, washed with water, dried over sodium sulfate and evaporated under reduced pressure. The resulting residue is purified by chromatography over aluminum oxide using chloroform for the elution. A by-product is first eluted and there is subsequently eluted the desired N,N-diethyl-N'-{dibenzo[b,e]thiepin-11(6H)-ylidene}-1,3-propanediamine-N'-oxide which is used directly in the process described in the first paragraph of this Example.

1. temperaturecooled to 5°-10° C
2. additionThe mixture is then treated dropwise with 15.3 g
3. customsubsequently evaporated under reduced pressure
4. dissolutionThe residue is dissolved in chloroform
5. washwashed with water
6. dry with materialdried over sodium sulfate
7. customevaporated under reduced pressure
8. customThe resulting residue is purified by chromatography over aluminum oxide
9. washfor the elution
10. washA by-product is first eluted
11. washthere is subsequently eluted the desired N,N-diethyl-N'-{dibenzo[b,e]thiepin-11(6H)-ylidene}-1,3-propanediamine-N'-oxide which