HCID 21923071、化合物 → HCID 178478851、化合物
反応式
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH2:8])[CH2:4][CH2:3]1.[Cl:9][C:10]1[N:18]=[C:17]2[C:13]([N:14]=[CH:15][N:16]2[CH:19]2[CH2:23][CH2:22][CH2:21][CH2:20]2)=[C:12]([NH:24][C:25]2[CH:33]=[CH:32][C:28]([C:29]([NH2:31])=[O:30])=[CH:27][CH:26]=2)[N:11]=1>O>[ClH:9].[ClH:9].[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:10]2[N:18]=[C:17]3[C:13]([N:14]=[CH:15][N:16]3[CH:19]3[CH2:20][CH2:21][CH2:22][CH2:23]3)=[C:12]([NH:24][C:25]3[CH:26]=[CH:27][C:28]([C:29]([NH2:31])=[O:30])=[CH:32][CH:33]=3)[N:11]=2)[CH2:4][CH2:3]1参加物
4
反応条件
- 温度
- 150 °C
実験手順
The operation is carried out as in Stage 2 of Example 6 and 800 mg of trans-1,4-diaminocyclohexane is introduced at ambient temperature under agitation then the reaction medium is heated at approximately 150° C. until melting and 249 mg of the product obtained in Stage 1 above is added, the reaction medium is left under agitation for 4 hours 30 minutes then left to return to ambient temperature. Then 10 ml of water is added, followed by extracting with 10 ml of methylene chloride containing 25% of methanol, drying, filtering, evaporating to dryness and taking up in 5 ml of ethanol. 2 ml of 1.4 N HCl in ethanol is added, followed by evaporating, leaving to crystallize, separating and washing with ethanol then drying at a temperature of approximately 60° C. In this way 207 mg of expected product is obtained in the form of colourless crystals.