Sodium Hydroxide → N-[2-[(4-Hydroxyphenyl)sulfonyl]ethyl]-2-propanamine hydrochloride
反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([CH2:12][CH2:13][NH:14][CH:15]([CH3:17])[CH3:16])(=[O:11])=[O:10])=[CH:5][CH:4]=1.[OH-:18].[Na+]>CS(C)=O>[ClH:2].[OH:18][C:3]1[CH:8]=[CH:7][C:6]([S:9]([CH2:12][CH2:13][NH:14][CH:15]([CH3:17])[CH3:16])(=[O:11])=[O:10])=[CH:5][CH:4]=1参加物
4
実験手順
A solution of N-[2-[(4-chlorophenyl)sulfonyl]ethyl]-1-methylethanamine hydrochloride and sodium hydroxide in 500 ml of dimethyl sulfoxide is heated at 95° C. for 2 hrs with stirring. The solvent is removed by rotary evaporation (vacuum pump) and the residue is partitioned between water (pH adjusted to 7 by the addition of dilute hydrochloric acid) and chloroform. The chloroform is removed and the residue is converted to the hydrochloride salt with ethereal hydrogen chloride. The salt is then recrystallized from methanol-diethyl ether to give crystalline title compound.
後処理
- customThe solvent is removed by rotary evaporation (vacuum pump)
- customthe residue is partitioned between water (
- additionpH adjusted to 7 by the addition of dilute hydrochloric acid) and chloroform
- customThe chloroform is removed
- customThe salt is then recrystallized from methanol-diethyl ether
出典と根拠
- ORDレコード
- ord-2823f427a751451592e29aeaf9842094
- 出典データセット
- uspto-grants-1986_07
- 特許番号
- US04597902
反応ノート
読み込み中…