反应详情

Dissolve 3 g (10.44 mmol) of 9-benzoylamino bicyclo[3.3.1]nonane-9-carboxylic acid in 200 mL of AcOH and 50 mL of 6N HCl aqueous solution, reflux the mixture for 18 h and then concentrate partially by distillation of 150 mL of solvent. After cooling, filter the reaction mixture and distribute in 150 mL of a 1:2 mixture of 1N HCl aqueous solution/ether. After extraction, concentrate the aqueous phase and then treat it dropwise with a 12N aqueous solution of soda (NaOH) to adjust the pH to 5-6. Filter the amino acid thus precipitated, wash with 3×50 mL of water and dry under reduced pressure, which gives 1.88 g of 9-aminobicyclo[3.3.1]nonane-9-carboxylic acid in the form of white crystals.

1. temperaturereflux the mixture for 18 h
2. concentrationconcentrate partially by distillation of 150 mL of solvent
3. temperatureAfter cooling
4. filtrationfilter the reaction mixture
5. additiondistribute in 150 mL of a 1:2 mixture of 1N HCl aqueous solution/ether
6. extractionAfter extraction
7. concentrationconcentrate the aqueous phase
8. additiontreat it dropwise with a 12N aqueous solution of soda (NaOH)
9. filtrationFilter the amino acid
10. customthus precipitated
11. washwash with 3×50 mL of water
12. customdry under reduced pressure, which