Reaction #710534
ord-c86ac210310144618949b44cd09a606b
Reaction equation
Methanesulfonic acid
(S)—N-(tert-butoxycarbonyl)-tert-leucine
triethylamine
→
titled compound
(S)-tert-leucine
Reagents
None
Solvents
Conditions
Temperature
25°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.
Workup
- 1Othera solid was precipitated
- 2OtherThe solid was sufficiently precipitated
- 3workup.STIRRINGthe solution was stirred at 25° C. for 30 minutes
- 4workup.STIRRINGfurther stirred at 25° C. for 30 minutes
- 5OtherThereafter, the solid was separated by filtration under reduced pressure
- 6WashThe solid was washed with methylene chloride (5 mL)
- 7Otherdrying
Procedure
Methanesulfonic acid (576 mg, 6 mmol) was added to a solution of (S)—N-(tert-butoxycarbonyl)-tert-leucine (1155 mg, 5 mmol) and methylene chloride (5 mL), and the mixture was stirred at 25° C. for 3 hours. When triethylamine (708 mg, 7 mmol) was added thereto, a solid was precipitated. The solid was sufficiently precipitated, and then the solution was stirred at 25° C. for 30 minutes and further stirred at 25° C. for 30 minutes. Thereafter, the solid was separated by filtration under reduced pressure. The solid was washed with methylene chloride (5 mL), and then was subjected to vacuum drying. Thereby, the titled compound was produced as a white solid (514 mg, yield of 75%).