反応式
[Cl:1][CH2:2][CH:3]([OH:16])[CH2:4][O:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:9]=[CH:8][CH:7]=1.[C:17]([CH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)#[N:18].Cl>O>[ClH:1].[C:17]([CH:19]1[CH2:24][CH2:23][N:22]([CH2:2][CH:3]([OH:16])[CH2:4][O:5][C:6]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH:9]=[CH:8][CH:7]=2)[CH2:21][CH2:20]1)#[N:18]参加物
実験手順
4.0 Parts of 1-chloro-3-(1-naphthoxy)-2-propanol and 16.0 parts of 4-cyanopiperidine are heated in a sealed vessel for 10 hours at about 100° C. That reaction mixture is then diluted with 50 parts of water, acidified with concentrated hydrochloric acid, and extracted with 35 parts of ethyl ether. The aqueous phase is separated and made alkaline with the addition of 10 N sodium hydroxide. The resultant solid is filtered and converted to the hydrochloride salt by redissolving the solid in isopropanol and adding a solution of hydrochloric acid in isopropanol. The resulting salt is separated by filtration and crystallized from a mixture of ethanol and ethyl ether to give 3-(4-cyanopiperidino)-1-(1-naphthoxy)-2-propanol hydrochloride, identical to the product of Example 1.
後処理
- extractionextracted with 35 parts of ethyl ether
- customThe aqueous phase is separated
- additionwith the addition of 10 N sodium hydroxide
- filtrationThe resultant solid is filtered
- dissolutionby redissolving the solid in isopropanol
- additionadding a solution of hydrochloric acid in isopropanol
- customThe resulting salt is separated by filtration
- customcrystallized from a mixture of ethanol and ethyl ether
出典と根拠
- ORDレコード
- ord-c3e7438776f746d28a1748cec81f8cac
- 出典データセット
- uspto-grants-1978_01
- 特許番号
- US04069221
関連ノート
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