反応式
[CH2:1]([N:3]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:4][CH2:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:10][CH:9]=1)[CH3:2].[BrH:26]>C(OCC)C>[BrH:26].[CH2:1]([N:3]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:4][CH2:5][CH2:6][CH2:7][C:8]1[CH:9]=[CH:10][C:11]([NH:14][S:15]([CH3:18])(=[O:16])=[O:17])=[CH:12][CH:13]=1)[CH3:2]参加物
4
実験手順
N-[4-[4-(ethylheptylamino)butyl]phenyl]methanesulfonamide (5.56 g, 0.015 mol), prepared according to the general procedure outlined in Example 1, was dissolved in diethyl ether. The solution was cooled with a dry ice/acetone bath and diethyl ether saturated with hydrogen bromide gas was added thereto. The volatiles were evaporated under reduced pressure and 100 ml of ethyl acetate was added to the residue. The solution was triturated and approximately 6 grams of crystals were collected. The solid was recrystalized from isopropyl alcohol to provide 2.5 g of N-[4-[4-(ethylheptylamino)butyl]phenyl]methanesulfonamide monohydrobromide. mp=98°-100° C. Yield 37%
後処理
- temperatureThe solution was cooled with a dry ice/acetone bath
- customThe volatiles were evaporated under reduced pressure and 100 ml of ethyl acetate
- additionwas added to the residue
- customThe solution was triturated
- customapproximately 6 grams of crystals were collected
- customThe solid was recrystalized from isopropyl alcohol
出典と根拠
- ORDレコード
- ord-70253ae8ff4f441392973bf47651d6ac
- 出典データセット
- uspto-grants-1986_06
- 特許番号
- US04596827
関連ノート
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