تفاعل #730238

معادلة التفاعل

(L)-tert-Leucine

NaOH

methyl chloroformate

→

title compound

المردود 98.0%

(2S)-2-[(methoxycarbonyl)amino]-3,3-dimethylbutanoic acid

المردود 98.0%

المذيبات

1,4-dioxane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled
2. 2
   استخلاصextracted twice with dichloromethane
3. 3
   أخرىThe aqueous layer was separated
4. 4
   درجة الحرارةcooled in ice bath
5. 5
   استخلاصThe mixture was extracted three times with ethyl acetate
6. 6
   أخرىthe organic layer was separated
7. 7
   تجفيفdried with sodium sulfate
8. 8
   ترشيحfiltered
9. 9
   أخرىthe solvents were evaporated

الإجراء التجريبي

(L)-tert-Leucine (10 g, 0.076 mol) was dissolved in 1,4-dioxane (40 mL) and treated with 2M NaOH (125 mL, 3.2 equivalents) followed by dropwise addition of methyl chloroformate (11.2 mL, 1.9 equivalents) at 25° C. The mixture was heated at 60° C. for 22 hrs, cooled, and extracted twice with dichloromethane. The aqueous layer was separated, cooled in ice bath, and acidified with 4N HCl (60 mL). The mixture was extracted three times with ethyl acetate, and the organic layer was separated, dried with sodium sulfate, filtered, and the solvents were evaporated to give 14.1 g (98%) of the title compound.

المصدر