反应详情

温度

0 °C

10.00 kg (29.81 mol, 1.0 eq) 3-[1-(phenylmethyl)-4-piperidinyl]-2,3,4,5-tetrahydro-1,3-benzodiazepin-2(1H)-one from Example 3 are dissolved in 100 L methanol, combined with 1.00 kg 10% Pd/C and hydrogenated in the pressurised reactor at 70° C. and 3 bar. After the hydrogen uptake has ended the catalyst is filtered off and washed with 30 L methanol. The filtrate is concentrated in vacuo and the residue is suspended in 100 L acetone. Then the mixture is refluxed, the suspension is stirred for 15 minutes at reflux temperature and half the acetone is distilled off at normal pressure. After the distillation has ended the mixture is cooled to 0° C. and stirred for a further hour. The product is suction filtered, washed with 20 L acetone and dried at 50° C.

1. filtrationis filtered off
2. washwashed with 30 L methanol
3. concentrationThe filtrate is concentrated in vacuo
4. temperatureThen the mixture is refluxed
5. temperatureat reflux temperature and half the acetone
6. distillationis distilled off at normal pressure
7. distillationAfter the distillation
8. stirringstirred for a further hour
9. filtrationfiltered
10. washwashed with 20 L acetone
11. customdried at 50° C.