反応式
[C:1]1([S:7]([CH2:10][CH2:11][Cl:12])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:13]([NH2:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(N(CC)CC)C>C(#N)C>[ClH:12].[C:1]1([S:7]([CH2:10][CH2:11][NH:20][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1参加物
5
実験手順
A mixture of 71.90 g (0.352 mole) of 2-chloroethyl phenyl sulfone, 37.45 g (0.350 mole) of benzylamine and 60 ml of triethylamine in 800 ml of acetonitrile was stirred at room temperature for ≈64 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the volume was reduced in vacuo to 300 ml. Methanol was added followed by an excess of ethereal hydrogen chloride. A white precipitate was collected to give 81.30 g (74.5%) of white, crystalline solid, m.p. 211°-213° C.
後処理
- customThe solvent was removed in vacuo
- customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
- dry with materialThe methylene chloride solution was dried over magnesium sulfate
- additionMethanol was added
- customA white precipitate was collected
- customto give 81.30 g (74.5%) of white, crystalline solid, m.p. 211°-213° C.
出典と根拠
- ORDレコード
- ord-81ada1811183440c81eed8afb7279bd4
- 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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