1-Methylpiperazine → Piperazine, 1-(3-butynyl)-4-methyl- (9CI)
反応式
CC1C=CC(S(O[CH2:12][CH2:13][C:14]#[CH:15])(=O)=O)=CC=1.[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C([O-])(O)=O.[Na+]>ClCCCl>[CH2:12]([N:20]1[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][CH2:19]1)[CH2:13][C:14]#[CH:15]参加物
5
反応条件
- 温度
- 70 °C
実験手順
A mixture of but-3-ynyl 4-methylbenzenesulfonate (972 mg) and N-methyl piperazine (482 μL) was heated to 80 C. for 4.5 h, diluted with 1,2-dichloroethane (5 mL) and heated to 70° C. for 18 h. Saturated aq. NaHCO3 was added (10 mL) and the mixture was extracted with DCM (3×40 mL), and concentrated to afford 0.70 g of 1-(but-3-ynyl)-4-methylpiperazine as a 3:2 mixture of tosylate salt and free base.
後処理
- temperaturewas heated to 80 C
- extractionthe mixture was extracted with DCM (3×40 mL)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-31a46f5b6acb446d8363e02483c1607d
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07544672B2
反応ノート
読み込み中…