L-Phenylalanine → HCID 22806804, compound

9.9 G (0.06 mol) of L-phenylalanine and 5.8 g (0.055 mol) of sodium carbonate were dissolved in 150 ml of water, into which 3.0 g (0.05 mol) of carbonyl sulfide was blown at a temperature of from 10° to 15° C. in 30 minutes. The mixture was then stirred for 30 minutes. To the mixture was added 6.3 g (0.05 mol) of benzylchloride dissolved in 90 ml of acetone dropwise in 15 minutes and the mixture was stirred for 2 hours at room temperature. After completion of the reaction, acetone was removed off from the solution by evaporating under reduced pressure. The residue was washed with 100 ml of benzene and the aqueous layer was acidified with concentrated hydrochloric acid to liberate an oily substance which was extracted twice with ethylacetate (each 100 ml). The ethylacetate layer was washed twice with water (each 100 ml) and was dried over anhydrous sodium sulfate. After drying, the drying agent was filtered. The filtrate was evaporated under reduced pressure to give a syrup-like substance which were added with 20 ml of ether and 50 ml of n-hexane. The mixed solution was stood in cold place to obtain 11.6 g of white powdery substance.

1. stirringthe mixture was stirred for 2 hours at room temperature
2. customwas removed off from the solution
3. customby evaporating under reduced pressure
4. washThe residue was washed with 100 ml of benzene
5. extractionwas extracted twice with ethylacetate (each 100 ml)
6. washThe ethylacetate layer was washed twice with water (each 100 ml) and
7. dry with materialwas dried over anhydrous sodium sulfate
8. customAfter drying
9. filtrationthe drying agent was filtered
10. customThe filtrate was evaporated under reduced pressure
11. customto give a syrup-like substance which
12. customto obtain 11.6 g of white powdery substance

ORD record

ord-acf4f34118364c3b93818c2a8cb1313f

Source dataset

uspto-grants-1979_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04138485