反应详情

35 mg (0.2 mmol) of 3-aminobenzenesulfonic acid and 57 mg (0.68 mmol) of sodium hydrogen carbonate were added to a mixed solvent of 2.0 ml of water and 0.5 ml of THF, and stirred at room temperature for 15 minutes. 20 μl (0.26 mmol) of thiophosgene was added and stirred at room temperature for another 40 minutes. Subsequently, 60 mg (0.2 mmol) of tert-butyl (2S)-3-amino-2-{[(tert-butoxy)carbonyl]amino}propanoate hydrochloride was added and stirred overnight. Following extraction with ethyl acetate, the solvent was distilled away, and 4.0 ml of trifluoroacetic acid was added to the residue, and the resultant was stirred at room temperature for 5 hours. After distilling the solvent away, purification step A was used to obtain 3.5 mg of the title compound.

1. stirringstirred at room temperature for another 40 minutes
2. stirringstirred overnight
3. extractionextraction with ethyl acetate
4. distillationthe solvent was distilled away
5. addition4.0 ml of trifluoroacetic acid was added to the residue
6. stirringthe resultant was stirred at room temperature for 5 hours
7. distillationAfter distilling the solvent away
8. custompurification step A