4-(Piperazin-1-yl)-2,6-di(pyrrolidin-1-yl)pyrimidine → HCID 69223635、化合物
反応式
[OH:1][C@H:2]1[CH2:22][CH2:21][C@@:20]2([CH3:23])[C:4](=[CH:5][CH2:6][C@@H:7]3[C@@H:19]2[CH2:18][CH2:17][C@@:16]2([CH3:24])[C@H:8]3[CH2:9][C@@H:10]([CH3:25])[C@@H:11]2[C:12](=[O:15])[CH2:13]I)[CH2:3]1.[N:26]1([C:31]2[N:36]=[C:35]([N:37]3[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]3)[CH:34]=[C:33]([N:43]3[CH2:47][CH2:46][CH2:45][CH2:44]3)[N:32]=2)[CH2:30][CH2:29][CH2:28][CH2:27]1>CN(C=O)C>[OH:1][C@H:2]1[CH2:22][CH2:21][C@@:20]2([CH3:23])[C:4](=[CH:5][CH2:6][C@@H:7]3[C@@H:19]2[CH2:18][CH2:17][C@@:16]2([CH3:24])[C@H:8]3[CH2:9][C@@H:10]([CH3:25])[C@@H:11]2[C:12](=[O:15])[CH2:13][N:40]2[CH2:41][CH2:42][N:37]([C:35]3[CH:34]=[C:33]([N:43]4[CH2:47][CH2:46][CH2:45][CH2:44]4)[N:32]=[C:31]([N:26]4[CH2:30][CH2:29][CH2:28][CH2:27]4)[N:36]=3)[CH2:38][CH2:39]2)[CH2:3]1参加物
4
実験手順
3β-Hydroxy-21-iodo-16α-methylpregn-5-en-20-one (10 g) is added all at once to 4-[2,6-bis(1-pyrrolidinyl)-4-pyrimidinyl]piperazine (16 g) in DMF (400 ml) at 65° and then concentrated to 50 ml under reduced pressure. The concentrate is added to sodium dihydrogen phosphate (0.3M, 400 ml) and ethyl acetate (500 ml). The pH is adjusted to 4.5 with 0.3M phosphoric acid. The ethyl acetate layer is separated and extracted with sodium dihydrogen phosphate (0.3M, 2×200 ml). The ethyl acetate extract is then washed with phosphoric acid (0.3M, 400 ml). The acid extract is stirred and the ph is adjusted to 3.5 with sodium hydroxide (10%). The resulting precipitate is filtered, washed with water (200 ml) and dried to give the title compound.