反応式
Cl.[CH3:2][C:3]1([CH3:31])[C:15]2[NH:14][C:13]3[C:8](=[CH:9][CH:10]=[C:11]([C:16]#[N:17])[CH:12]=3)[C:7]=2[C:6](=[O:18])[C:5]2[CH:19]=[CH:20][C:21]([O:23][CH2:24][CH:25]3[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]3)=[CH:22][C:4]1=2.[O:32]1[CH2:35][C:34](=O)[CH2:33]1.C1COCC1.C([BH3-])#N.[Na+]>C(O)(=O)C.O.CO>[CH3:2][C:3]1([CH3:31])[C:15]2[NH:14][C:13]3[C:8](=[CH:9][CH:10]=[C:11]([C:16]#[N:17])[CH:12]=3)[C:7]=2[C:6](=[O:18])[C:5]2[CH:19]=[CH:20][C:21]([O:23][CH2:24][CH:25]3[CH2:30][CH2:29][N:28]([CH:34]4[CH2:35][O:32][CH2:33]4)[CH2:27][CH2:26]3)=[CH:22][C:4]1=2参加物
8
反応物 4
生成物 1
試薬・触媒・溶媒 3
実験手順
6,6-Dimethyl-11-oxo-8-(piperidin-4-ylmethoxy)-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile hydrochloric acid salt (Compound A7-25, 30 mg, 0.075 mmol) and oxetan-3-one (38 mg, 7 eq.) were dissolved in acetic acid (0.2 ml), THF (1 ml) and methanol (1 ml), added with sodium cyanoborohydride (33 mg, 7 eq.) at room temperature, and stirred overnight. The reaction solution was added with water, and then extracted with ethyl acetate. The solution was dried over sodium sulfate and the solvent was removed under vacuum and the resulting residues were purified by preparative TLC (chloroform: 2 N ammonia methanol=9:1) to obtain the target compound (15 mg).
後処理
- extractionextracted with ethyl acetate
- dry with materialThe solution was dried over sodium sulfate
- customthe solvent was removed under vacuum
- customthe resulting residues were purified by preparative TLC (chloroform: 2 N ammonia methanol=9:1)
出典と根拠
- ORDレコード
- ord-b18223b5a281405fb046a292826eac0a
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440922B2
関連ノート
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