反应详情

7.5 ml of a Raney nickel suspension is washed four times with respectively 30 ml of methanol. Then 15 ml of methanol and thereafter a solution of 670 mg (1.5 mmol) of 1,1-diethyl-3-[2-(1,3-dithiolan-2-yl)-6-methyl-8α-ergolinyl]urea in 15 ml of methanol are added thereto. The mixture is agitated for 3 hours at room temperature and once again 7.5 ml of a Raney nickel suspension is added which has been washed, as above, previously four times with respectively 30 ml of methanol. After another 2 hours of agitation at room temperature, the catalyst is filtered off over a silica gel column and thoroughly washed with methanol. The filtrate is evaporated and the residue is crystallized from methanol/ethyl acetate, thus obtaining 170 mg of 1,1-diethyl-3-(2,6-dimethyl-8α-ergolinyl)urea (32% yield).

1. wash7.5 ml of a Raney nickel suspension is washed four times with respectively 30 ml of methanol
2. washhas been washed
3. waitAfter another 2 hours of agitation at room temperature
4. filtrationthe catalyst is filtered off over a silica gel column
5. washthoroughly washed with methanol
6. customThe filtrate is evaporated
7. customthe residue is crystallized from methanol/ethyl acetate