HRID1906588
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A 500 ml steel autoclave was loaded in a glove box (O2 -content less than 1 ppm) with 40.0 g (0.31 mol) of ketopantolactone, 210 ml of toluene, 180.6 mg (0.389 mmol) of [Rh(COD)2 ]PF6, 237.3 mg (0.389 mmol) of mCH3 --BPPM and 138.3 mg (0.389 mmol) of tetrabutylammonium trifluoroacetate. The hydrogenation was carried out at a constant pressure of 40 bar of H2 at 30° C. and with intensive stirring. By virtue of the exothermic reaction the temperature rose to 55° C. A conversion of above 99% was achieved after 1.2 hours. After a total hydrogenation time of 2 hours the mixture was worked-up as described in Example 2. Pure (R)-pantolactone was obtained. [α]D20 =-46.0°. Optical purity 89.1%.
WORKUP
后处理
- customwas carried out at a constant pressure of 40 bar of H2 at 30° C. and with intensive stirring
- customBy virtue of the exothermic reaction the temperature
- customrose to 55° C
- customAfter a total hydrogenation time of 2 hours