تفاعل #1427

معادلة التفاعل

Potassium bromide

D-leucine

sodium nitrite

→

crude title product

(S)-2-Bromo-4-methylpentanoic acid

المذيبات

sulfuric acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةmaintaining the temperature between -10° and -5° C
2. 2
   workup.ADDITIONAfter addition
3. 3
   درجة الحرارةwarmed to room temperature
4. 4
   workup.STIRRINGstirred for another hour
5. 5
   استخلاصThe reaction mixture was then extracted twice with ether
6. 6
   غسيلthe ether extracts were washed once with water
7. 7
   تجفيفdried (magnesium sulfate)
8. 8
   ترشيحfiltered
9. 9
   أخرىevaporated
10. 10
    أخرىto give 2.7 g

الإجراء التجريبي

Potassium bromide (9.5 g., 80 mmol.) was added to a stirred solution of D-leucine (3.0 g., 23 mmol.) in 2.5N sulfuric acid (47 ml.) at room temperature. The reaction mixture was cooled to -10° C. and solid sodium nitrite (2.4 g., 34 mmol.) was added portionwise, maintaining the temperature between -10° and -5° C. After addition was complete, the reaction was stirred for 1 hour and then warmed to room temperature and stirred for another hour. The reaction mixture was then extracted twice with ether, the ether extracts were washed once with water, dried (magnesium sulfate), filtered and evaporated to give 2.7 g. of crude title product.

المصدر