反応式
[ClH:1].[CH3:2][CH:3]([NH:5][CH2:6][CH2:7][S:8][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=1)[CH3:4].B1([O-])O[O:20]1.O.O.O.O.[Na+].[OH-].[Na+]>S(=O)(=O)(O)O>[ClH:1].[CH3:4][CH:3]([NH:5][CH2:6][CH2:7][S:8]([C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=1)=[O:20])[CH3:2]参加物
5
実験手順
A solution of 12.0 g (0.043 mole) of 1-methyl-N-[2-(1-naphthalenylthio)ethyl]ethanamine hydrochloride and 19.7 g (0.028 mole) of sodium perborate tetrahydrate in 500 ml of 2N sulfuric acid was stirred overnight at room temperature. The solution was poured over ice and the mixture was made alkaline with 50% sodium hydroxide and then extracted with chloroform. The chloroform layer was evaporated to give a dark-brown oil, the free base of the title compound, which crystallized at room temperature. A one gram sample was reacted with ethereal hydrogen chloride and recrystallized from methanol-diethyl ether to give 0.72 g (9.1%) of white solid, m.p. 153°-155° C.
後処理
- additionThe solution was poured over ice
- extractionextracted with chloroform
- customThe chloroform layer was evaporated
- customto give a dark-brown oil
- customthe free base of the title compound, which crystallized at room temperature
- customA one gram sample was reacted with ethereal hydrogen chloride
- customrecrystallized from methanol-diethyl ether
出典と根拠
- ORDレコード
- ord-c0e824ff2ea84ee0a559f8efc8f63b92
- 出典データセット
- uspto-grants-1988_02
- 特許番号
- US04724235
関連ノート
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