反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.[C:15]([OH:25])(=[O:24])[C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[CH2:17]>C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:17][CH:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:15]([OH:25])=[O:24])[CH2:11][CH2:10]1参加物
4
実験手順
1-(2-Methoxyphenyl)piperazine (22.6 g; 0.118 mol) and atropic acid (174 g, 0.118 moll in ethanol (300 ml) were heated under reflux for 18 hours, cooled to room temperature, and evaporated in vacuo. The solid was triturated with acetone (3×100 ml) to give a first crop of product (13.8 g) as white crystals. The filtrate was evaporated in vacuo to give an oil which slowly crystallised over 1 month. The solid was triturated with acetone (200 ml) to give a second crop of the hemihydrate of the product (9.01 g) as white crystals, m.p. 160°-163°. (Found: C, 68.4; H, 7.2; N, 7.9. C20H24N2O3.0.5H2O requires C, 68.8; H, 7.2; N, 8.0%.)
後処理
- temperatureunder reflux for 18 hours
- customevaporated in vacuo
- customThe solid was triturated with acetone (3×100 ml)
出典と根拠
- ORDレコード
- ord-ccae9be3c5eb46ebbf97353a9823ff7c
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05420278
関連ノート
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