反应详情

86 g of methyl 5-chloro-3-(1,3-dioxolan-2-yl)-2-hydroxybenzoate are dissolved in a mixture of 700 ml of methanol and 50 ml of tetrahydrofuran, and 70 ml of triethylamine and 7 g of 10% palladium-carbon are added to the solution. The mixture is subjected to catalytic hydrogenation under atmospheric pressure. The reaction mixture is filtered and the filtrate is evaporated to remove solvent. 10% hydrochloric acid is added to the residue and the mixture is concentrated. Water is added to the residue and the aqueous mixture is extracted with ethyl acetate. The extract is dried and evaporated to remove solvent. The resultant crystals are collected, washed with cold ethanol and dried to give 51.1 g of methyl 3-formyl-2-hydroxybenzoate as colorless needles.

1. additionare added to the solution
2. filtrationThe reaction mixture is filtered
3. customthe filtrate is evaporated
4. customto remove solvent
5. addition10% hydrochloric acid is added to the residue
6. concentrationthe mixture is concentrated
7. additionWater is added to the residue
8. extractionthe aqueous mixture is extracted with ethyl acetate
9. customThe extract is dried
10. customevaporated
11. customto remove solvent
12. customThe resultant crystals are collected
13. washwashed with cold ethanol
14. customdried