反应详情

To an ice-cooled solution of 4-(2-chlorophenyl)-2-(2,3-dihydroxypropoxymethyl)-1,4-dihydro-6-methyl-3,5-pyridinedicarboxylic acid 3-ethyl 5-methyl ester (IC, 13.0 g) in methanol (150 mL) was added a solution of sodium periodate (7.6 g) dissolved in water (100 mL) dropwise over 15 min. After stirring for 10 min, a saturated solution of ammonium chloride (25 mL) was added. Volatile materials were removed under reduced pressure, then ethyl acetate (200 mL) and water (100 mL) were added. The organic layer was separated and the aqueous layer was twice extracted with ethyl acetate (50 mL). The combined organic fractions was washed with brine, dried (sodium sulfate), filtered and concentrated in vacuo to afford the title compound (11.8 g). Thin layer chromatography and proton NMR spectrum showed the crude title compound (ID) was sufficiently pure.

1. customVolatile materials were removed under reduced pressure
2. additionethyl acetate (200 mL) and water (100 mL) were added
3. customThe organic layer was separated
4. extractionthe aqueous layer was twice extracted with ethyl acetate (50 mL)
5. washThe combined organic fractions was washed with brine
6. dry with materialdried (sodium sulfate)
7. filtrationfiltered
8. concentrationconcentrated in vacuo