反应详情

7.5 ml of a Raney nickel suspension is washed four times with respectively 30 ml of methanol. Thereafter, 15 ml of methanol and then a solution of 690 mg (1.5 mmol) of 1,1-diethyl-3-[2-(1,3-dithiolan-2-yl)-1,6-dimethyl-8α-ergolinyl]urea in 15 ml of methanol are added thereto. The mixture is agitated for 3 hours at room temperature and then once more 7.5 ml of a Raney nickel suspension, previously washed as above four times with respectively 30 ml of methanol, is added thereto. After another 2 hours of agitation at room temperature, the catalyst is filtered off via a silica gel column and washed thoroughly with methanol. The filtrate is evaporated and the residue crystallized from methanol/ethyl acetate, thus obtaining 150 mg of 1,1-diethyl-3-(1,2,6-trimethyl8α-ergolinyl)urea (27% yield).

1. wash7.5 ml of a Raney nickel suspension is washed four times with respectively 30 ml of methanol
2. washonce more 7.5 ml of a Raney nickel suspension, previously washed as above four times with respectively 30 ml of methanol
3. additionis added
4. waitAfter another 2 hours of agitation at room temperature
5. filtrationthe catalyst is filtered off via a silica gel column
6. washwashed thoroughly with methanol
7. customThe filtrate is evaporated
8. customthe residue crystallized from methanol/ethyl acetate