Reaktion #710534

Reaktionsgleichung

Methanesulfonic acid

(S)—N-(tert-butoxycarbonyl)-tert-leucine

triethylamine

→

titled compound

(S)-tert-leucine

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigea solid was precipitated
2. 2
   SonstigeThe solid was sufficiently precipitated
3. 3
   workup.STIRRINGthe solution was stirred at 25° C. for 30 minutes
4. 4
   workup.STIRRINGfurther stirred at 25° C. for 30 minutes
5. 5
   SonstigeThereafter, the solid was separated by filtration under reduced pressure
6. 6
   WaschenThe solid was washed with methylene chloride (5 mL)
7. 7
   Sonstigedrying

Vorschrift

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%).

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