Into a pressurised vessel containing nitrogen is put 4-methylene-2-oxetanone, a solvent (not an alcohol or water), e.g. methylene chloride, and 0.0001 to 0.1 mol per mol of the oxetanone of a catalyst prepared by mixing ruthenium with an optically active phosphine compound in a molar ratio of 1:1 to 1:0.95 so as to make a complex, hydrogen is passed at a pressure of 5 to 150 kg/cm² at room temperature to 100°C for 15 to 150 hours, so as to prepare optically active 4-methyl-2-oxetanone.
Preferably a tertiary amine is also present which is added to the catalyst and solvent before addition of the oxetanone.
Seven classes of catalytic complexes are described, with their preparations.
The product is obtained in high yield and high optical purity and is useful as an intermediate in syntheses.
将 4-亚甲基-2-氧杂
环丁酮、溶剂(非
酒精或
水)(如
二氯甲烷)和每摩尔氧杂
环丁酮 0.0001 至 0.1 摩尔的催化剂(将
钌与具有光学活性的膦化合物按 1:1 至 1:0 的摩尔比混合制备)放入盛有氮气的加压容器中,然后在室温至 100°C 下以 5 至 150 千克/平方厘米的压力通入
氢气 15 至 150 小时,以制备具有光学活性的 4-亚甲基-2-氧杂
环丁酮。95 制成络合物,在室温至 100℃、压力为 5 至 150 千克/平方厘米的条件下通入
氢气 15 至 150 小时,以制备光学活性的 4-甲基-2-氧杂
环丁酮。
在加入氧杂
环丁酮之前,最好还在催化剂和溶剂中加入叔胺。
本文介绍了七类催化络合物及其制备方法。
该产品收率高、光学纯度高,可用作合成的中间体。