反応式
C[O:2][C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][N:13]([CH3:16])[CH2:12][CH2:11]2)=[CH:6][CH:5]=1.[ClH:18]>CC(C)=O>[ClH:18].[CH3:16][N:13]1[CH2:12][CH2:11][N:10]([C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:17])=[O:2])=[CH:5][CH:6]=2)[CH2:15][CH2:14]1参加物
4
反応条件
- 温度
- 2 °C
実験手順
4-(4-Methyl-piperazin-1-yl)-benzoic acid methyl ester (8.5 mmol) is dissolved in 4N HCl (15 ml) and heated under reflux for 8 hours. The mixture is cooled in an ice bath to 0-4° C., diluted with 5 ml acetone and the solid material formed is filtered off, washed with acetone and dried (vacuum). A white powder with mp. >270° C., Rf=0.11 (CH2Cl2/MeOH=9:1) is obtained.
後処理
- temperatureheated
- temperatureunder reflux for 8 hours
- customthe solid material formed
- filtrationis filtered off
- washwashed with acetone
- customdried (vacuum)
- customA white powder with mp. >270° C., Rf=0.11 (CH2Cl2/MeOH=9:1) is obtained
出典と根拠
- ORDレコード
- ord-e05871aee5d34ade99a6fdea2466975f
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06642239B2
関連ノート
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