Methane → Zeranol

反応式

[CH2:1]1[CH2:19][CH2:18][C:17]2[C:12](=[C:13]([OH:21])[CH:14]=[C:15]([OH:20])[CH:16]=2)[C:10](=[O:11])[O:9][CH2:8][CH2:7][CH2:6][CH2:5][C@@H:4]([OH:22])[CH2:3][CH2:2]1.[C:23](#N)C.C>O>[CH3:23][C@@H:8]1[O:9][C:10](=[O:11])[C:12]2[C:17](=[CH:16][C:15]([OH:20])=[CH:14][C:13]=2[OH:21])[CH2:18][CH2:19][CH2:1][CH2:2][CH2:3][C@@H:4]([OH:22])[CH2:5][CH2:6][CH2:7]1

参加物

実験手順

3 59 kg of an α, β-zeranol mixture (55:45), acetonitrile with 0.5% water (80 1) and active charcoal (0.05 kg) were placed into a 150 1 crystallizer. The mixture was refluxed for 30 min., warm filtered and the filtrate was refluxed again. The obtained clear solution was cooled adjusting the fall in temperature to about 8°-10° C./hour, under strong mechanic stirring, so as to obtain a controlled crystallization. Crystal withdrawals were carried out at 42° C., 36° C. and 30° C. on which crystals HPLC analysis was effected a described in Example 1: content in α-zeranol proved to be extremely constant (9I.9%, 92.3% and 9I.8%, respectively, at the above cited temperatures). Stirring was continued overnight and for I2 hours more at 30 C; then the product was filtered and dried to obtain 1.40 kg (38.99%) of an α-zeranol with a 93.5% titre. This product was dissolved in 42 1 of acetonitrile with 1% of water and crystallized following the same procedure as above. 1.01 kg of final product was obtained, with a 98.6% titre (HPLC), m.p.=181°-182° C., [α]D20 =46.2 (c =1.0; methanol).