反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]([O:10]O)=[O:9])[CH:3]=1.CC(N1CCOCC1)(C)C(C1C=CC(SC)=CC=1)=O>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[C:8]([OH:10])=[O:9]参加物
4
実験手順
A solution of 13 g of m-chloroperbenzoic acid in 50 g of CH2Cl2 is added dropwise, at 0° and while stirring, to a solution of 20 g of 2-methyl-1-[4-(methylthio)phenyl]-2-morpholinopropan-1-one in 200 g of methylene chloride. Stirring is continued for a further 2 hours, in the course of which the m-chlorobenzoic acid formed is deposited in the form of a white precipitate. The reaction mixture is poured into ice/1N NaOH, and the organic phase is separated off, dried over Na2SO4 and evaporated on a rotary evaporator. The crude 2-methyl-1-[4-(methylsulfenyl)phenyl]-2-morpholinopropan-1-one which remains is recrystallised from ethyl acetate/hexane. Melting point 112°-113° C. (Compound No. 31).
出典と根拠
- ORDレコード
- ord-0e4bb4809ec44e33b36b76361a0c9829
- 出典データセット
- uspto-grants-1986_04
- 特許番号
- US04582862
関連ノート
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