Methanesulfonic Acid → HCID 13760254、化合物
反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][C:19]=1[O:20][CH3:21])[CH2:6][NH:7][CH2:8][CH:9](O)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CS(O)(=O)=O>ClCCl>[CH3:21][O:20][C:19]1[CH:18]=[C:17]2[C:5](=[CH:4][C:3]=1[O:2][CH3:1])[CH2:6][NH:7][CH2:8][CH:9]2[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1参加物
4
実験手順
Add the amino-alcohol from step A (2.2 g) to a mixture of methanesulfonic acid (100 mL) and dichloromethane (150 mL) and stir overnight at room temperature. Pour the mixture into ice-water, separate and concentrate the organic layer to a residue. Triturate with benzene then recrystallize from ethanol to give 8.7 g of the title amine as the methanesulfonate salt, mp=198°-199° C.
後処理
- customseparate
- concentrationconcentrate the organic layer to a residue
- customTriturate with benzene
- customthen recrystallize from ethanol
出典と根拠
- ORDレコード
- ord-b31db5b93fa64d7694624aa086bdacb7
- 出典データセット
- uspto-grants-1992_06
- 特許番号
- US05124337
反応ノート
読み込み中…