反応 #1427

反応方程式

Potassium bromide

D-leucine

sodium nitrite

→

crude title product

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

溶媒

sulfuric acid

反応条件

後処理

1. 1
   温度maintaining the temperature between -10° and -5° C
2. 2
   workup.ADDITIONAfter addition
3. 3
   温度warmed to room temperature
4. 4
   workup.STIRRINGstirred for another hour
5. 5
   抽出The reaction mixture was then extracted twice with ether
6. 6
   洗浄the ether extracts were washed once with water
7. 7
   乾燥dried (magnesium sulfate)
8. 8
   ろ過filtered
9. 9
   その他evaporated
10. 10
    その他to give 2.7 g

実験手順

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.

出典