反応式
C([Li])CCC.[CH2:6]([OH:9])[C:7]#[CH:8].Cl[C:11]([N:13]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[C:17](=[O:24])[NH:16][C:15]2[CH:25]=[CH:26][CH:27]=[N:28][C:14]1=2)=[O:12]>CCCCCC.O1CCCC1>[CH2:6]([O:9][C:11]([N:13]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[C:17](=[O:24])[NH:16][C:15]2[CH:25]=[CH:26][CH:27]=[N:28][C:14]1=2)=[O:12])[C:7]#[CH:8]参加物
6
実験手順
At 15° to 20° C., 3.08 g (0.048 mol) of n-butyl-lithium in 30 ml of n-hexane are added dropwise to a solution of 2.24 g (0.04 mol) of propargyl alcohol in 120 ml of tetrahydrofuran. After it has all been added, the mixture is stirred for a further 30 minutes at ambient temperature and then mixed with a suspension of 10.9 g (0.04 mol) of 11-chlorocarbonyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one in 250 ml of tetrahydrofuran. In order to complete the reaction the mixture is stirred for a further hour. It is evaporated to dryness in vacuo and the residue is crystallised by stirring in water. After recrystallisation from ethyl acetate, 7.5 g (64% of theory) of the desired product are obtained, m.p. 213° C.
後処理
- additionall been added
- customthe reaction the mixture
- stirringis stirred for a further hour
- customIt is evaporated to dryness in vacuo
- customthe residue is crystallised
- stirringby stirring in water
- customAfter recrystallisation from ethyl acetate, 7.5 g (64% of theory) of the desired product
- customare obtained
出典と根拠
- ORDレコード
- ord-b62934e97d654247b2961e7c9f60d869
- 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…