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    • 5. 发明申请
    • Process for preparing solutions of alkali metal salts of functionalized alcohols
    • 制备官能醇的碱金属盐溶液的方法
    • US20040097759A1
    • 2004-05-20
    • US10704808
    • 2003-11-12
    • DEGUSSA AG
    • Johannes RuwweKlaus Stadtmueller
    • C07C323/10C07F001/02C07C031/34
    • C07C213/08C07C215/08
    • Alkali metal salt of formula (I): MOYXR1 (I), and its solution can be prepared in high yields, particularly high space-time yields, and with high purities by reacting an alcohol of the formula (Ia): HOYXR1 (Ia), in a solvent mixture with an alkali metal salt of formula (II): MOR2 (II), or by reacting the alcohol (Ia) in a solvent mixture with an alkali metal hydroxide. Part of the liberated alcohol of formula (IIa): HOR2 (IIa) or a part of the liberated water is distilled from the solvent mixture, initially, without addition of an entrainer. Subsequently, a remainder of the liberated alcohol of formula (IIa) or the liberated water is distilled from the solvent mixture with the aid of at least one organic solvent as entrainer. In formula (I) and in formula (II), M is Li, Na, K, Rb or Cs. In formula (I) and in formula (Ia): Y is (C1-C8)-alkylene, X is O, S or NR1, and R1 is H, (C1-C8)-alkyl, (C2-C8)-alkenyl, (C2-C8)-alkynyl, (C3-C8)-cycloalkyl, (C6-C18)-aryl, (C7-C19)-aralkyl, (C3-C18)-heteroaryl, (C4-C19)-heteroaralkyl, ((C1-C8)-alkyl)1-3-(C3-C8)-cycloalkyl, ((C1-C8)-alkyl)1-3-(C6-C18)-aryl or ((C1-C8)-alkyl)1-3-(C3-C18)-heteoraryl. In formula (II) and in formula (IIa), R2 is methyl, ethyl, propyl, isopropyl, sec-butyl, isobutyl or tert-butyl.
    • 式(I)的碱金属盐:MOYXR 1(I),其溶液可以以高产率,特别高的时空产率制备,并且通过使式(Ia)的醇:HOYXR (Ia)中,在与式(II)的碱金属盐:MOR 2(II)的溶剂混合物中,或通过使溶剂混合物中的醇(Ia)与碱金属氢氧化物反应。 一部分式(IIa)的游离醇:HOR 2(IIa)或部分释放的水最初从溶剂混合物中蒸馏,不加入夹带剂。 随后,借助于至少一种有机溶剂作为夹带剂,将溶剂式(IIa)的游离醇的余量或释放的水从溶剂混合物中蒸馏出。 在式(I)和式(II)中,M是Li,Na,K,Rb或Cs。 在式(I)和式(Ia)中:Y是(C 1 -C 8) - 亚烷基,X是O,S或NR 1,R 1是H,(C 1 -C 8) - 烷基,( (C 2 -C 8) - 烯基,(C 2 -C 8) - 炔基,(C 3 -C 8) - 环烷基,(C 6 -C 18) - 芳基,(C 7 -C 19) - 芳烷基,(C 3 -C 18) ((C 1 -C 8) - 烷基)1-3 - (C 3 -C 8) - 环烷基,((C 1 -C 8) - 烷基)1-3 - (C 6 -C 18) - 芳基或((C 1 -C 8) -C 8) - 烷基)1-3 - (C 3 -C 18) - 杂芳基。 在式(II)和式(IIa)中,R 2是甲基,乙基,丙基,异丙基,仲丁基,异丁基或叔丁基。