反応式
[Cl:1]CCCO[CH:6]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[NH:8][C:7]1=[O:16].[CH3:17][O:18][C:19]1[CH:20]=[C:21]([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)[CH:22]=[C:23]([O:27][CH3:28])[C:24]=1[O:25][CH3:26].[C:35](=[O:38])([O-])O.[Na+].[ClH:40].[CH2:41](O)[CH3:42]>CS(C)=O.N1C=CC=CC=1>[ClH:1].[ClH:40].[CH3:28][O:27][C:23]1[CH:22]=[C:21]([N:29]2[CH2:34][CH2:33][N:32]([CH2:41][CH2:42][CH2:35][O:38][C:11]3[CH:10]=[C:9]4[C:14]([CH2:15][CH2:6][C:7](=[O:16])[NH:8]4)=[CH:13][CH:12]=3)[CH2:31][CH2:30]2)[CH:20]=[C:19]([O:18][CH3:17])[C:24]=1[O:25][CH3:26]参加物
反応物 5
生成物 1
試薬・触媒・溶媒 2
実験手順
12.4 grams of 7-(3-chloropropoxy-3,4-dihydrocarbostyril, 1 g of pyridine and 2.6 g of 4-(3,4,5-trimethoxyphenyl)piperazine are mixed in 20 ml of dimethylsulfoxide, then stirred at 80°-90° C. for 5 hours. The reaction mixture is poured into 80 ml of 2% aqueous solution of sodium hydrogencarbonate and the organic layer is extracted with chloroform. The chloroform layer is washed with water, dried and chloroform is removed by distillation. The residue thus obtained is dissolved in 30 ml of ethanol and dried hydrogen chloride gas is blown into the ethanol solution. The crystals thus precipitated are collected by filtration and recrystallized from methanol-ethanol to obtain 3.2 g (yield: 61%) of 7-{3-[4-(3,4,5-trimethoxyphenyl)-piperazinyl]propoxy}-3,4-dihydrocarbostyril dihydrochloride in the form of colorless needle-like crystals with a melting point of 225°-227° C.
後処理
- extractionthe organic layer is extracted with chloroform
- washThe chloroform layer is washed with water
- customdried
- customchloroform is removed by distillation
- customThe residue thus obtained
- customThe crystals thus precipitated
- filtrationare collected by filtration
- customrecrystallized from methanol-ethanol
出典と根拠
- ORDレコード
- ord-6c25e9bb8ead4005a472cd4def0bbcbc
- 出典データセット
- uspto-grants-1989_04
- 特許番号
- US04824840
関連ノート
読み込み中…