反応式
[O:1]=[C:2]([N:7]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[C:11](=[O:18])[NH:10][C:9]2[CH:19]=[CH:20][CH:21]=[N:22][C:8]1=2)[CH2:3][CH2:4][C:5]#[CH:6].[CH2:23]=O.[NH:25]1[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1>[Cu]Cl.O1CCOCC1>[O:1]=[C:2]([N:7]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[C:11](=[O:18])[NH:10][C:9]2[CH:19]=[CH:20][CH:21]=[N:22][C:8]1=2)[CH2:3][CH2:4][C:5]#[C:6][CH2:23][N:25]1[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
A mixture consisting of 9.6 g (0.03 mol) of 5,11-dihydro-11-[1-oxo-4-pentynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 1.08 g (0.036 mol) of paraformaldehyde, 3.06 g (0.036 mol) of piperidine, 0.2 g of copper(I) chloride and 150 ml of dioxan is refluxed for 1 hour. After the reaction has ended the insoluble constituents are filtered off and the filtrate is evaporated to dryness in vacuo. The crude product is purified by column chromatography on silica gel (mobile phase: ethyl acetate, ethyl acetate+10% methanol). After recrystallisation from ethyl acetate, 2.7 g (21% of theory) of the desired compound are obtained, m.p. 197° C.
後処理
- temperatureis refluxed for 1 hour
- filtrationare filtered off
- customthe filtrate is evaporated to dryness in vacuo
- customThe crude product is purified by column chromatography on silica gel (mobile phase: ethyl acetate, ethyl acetate+10% methanol)
- customAfter recrystallisation from ethyl acetate, 2.7 g (21% of theory) of the desired compound
- customare obtained
出典と根拠
- ORDレコード
- ord-301ed65de99248bebe2bd6e6ac674570
- 出典データセット
- uspto-grants-1988_02
- 特許番号
- US04724236
関連ノート
読み込み中…