反应详情

5.8 ml of 95% sulfuric acid was added to 33 ml of methanol and heat-refluxed. Subsequently, methanol was removed under reduced pressure and water was added to provide 15 ml of CH3SO4H solution. 2.7 g L-Phe and 0.3 g (D-Phe/L-Phe=11.1%) D-Phe were added thereto and dissolved by heat, following which was then cooled with ice. The separated crystals were isolated by suction filtration and washed with a small amount of cold water. Yield, 3.73 g. The results of HPLC analysis using an optically active column revealed that the crystals contained 1.66 g L-Phe and 0.049 g (D-Phe/L-Phe=2.9%) D-Phe. In addition, 41 mg of L-phenylalanine methyl ester was also produced as a result of esterification of L-Phe with the methanol remaining in the CH3SO4H solution.

1. temperatureheat-refluxed
2. customSubsequently, methanol was removed under reduced pressure and water
3. additionwas added
4. customto provide 15 ml of CH3SO4H solution
5. dissolutiondissolved
6. temperatureby heat
7. temperaturewas then cooled with ice
8. customThe separated crystals were isolated by suction filtration
9. washwashed with a small amount of cold water
10. customYield
11. customThe results of HPLC analysis