[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](N3CCOCC3)=[C:9]([C:19](=[S:22])[NH:20][CH3:21])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.[OH2:24]>C(O)C>[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](=[O:24])[CH:9]([C:19](=[S:22])[NH:20][CH3:21])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]11 g of 4-cyclohexyl 2-methylthiocarbamoyl 1-morpholyl cyclohex-1 ene is dissolved in 20 ml ethanol at room temperature. To this solution 2 ml 4 N hydrochloric acid solution are added and the mixture becomes pale yellow. The reaction mixture is kept under stirring for 1/2 hour. 60 ml water are then added and a brownish-red precipitate appears. It is sucction-filtered, washed with water and further taken up in benzene until complete solution. The benzenic solution is dried, filtered and evaporated to dryness. The dry residue is further washed with water then taken up with benzene. After distillation of the solvent 0.7 g of 4-cyclohexyl 2-methyl thio carbamoyl cyclohexanone are thus obtained which is used as such for the next step of the synthesis.
Loading…