Sodium Bicarbonate → 86287-91-4

20 g (0.085 mol) methyl 2-chloroethyl cysteine hydrochloride was dissolved with 200 ml water, and a solution of 7.2 g (0.085 mol) sodium bicarbonate dissolved in 120 ml water was added dropwise to the above-obtained solution under ice bath condition, and then the mixed solution was allowed to react by keeping a constant temperature in the bath ice for 1 hour. The obtained reaction product was extracted with ethyl acetate (100 ml×3), and the resulting ester layers were combined, and dried with anhydrous sodium sulfate for 4 hours. The solvent was removed by evaporation under reduced pressure. The resulting residue was dissolved with 400 ml anhydrous methanol, and reacted with stirring at room temperature for 5 days, followed by removing solvent by evaporation under reduced pressure. The resulting residue was recrystallized with anhydrous methanol/ethyl acetate, obtaining 8.9 g of a white crystal, yield 49.2%.

1. additionwas added dropwise to the above-obtained solution under ice bath condition
2. customto react
3. customfor 1 hour
4. customThe obtained reaction product
5. extractionwas extracted with ethyl acetate (100 ml×3)
6. dry with materialdried with anhydrous sodium sulfate for 4 hours
7. customThe solvent was removed by evaporation under reduced pressure
8. dissolutionThe resulting residue was dissolved with 400 ml anhydrous methanol
9. customreacted
10. customby removing solvent
11. customby evaporation under reduced pressure
12. customThe resulting residue was recrystallized with anhydrous methanol/ethyl acetate

ORD record

ord-1f169456011f4d2a9d5f048b59f212ad

Source dataset

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08173643B2