反应 #1427

反应方程式

Potassium bromide

D-leucine

sodium nitrite

→

crude title product

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

溶剂

sulfuric acid

反应条件

后处理

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
   萃取The reaction mixture was then extracted twice with ether
6. 6
   洗涤the ether extracts were washed once with water
7. 7
   干燥dried (magnesium sulfate)
8. 8
   过滤filtered
9. 9
   其他evaporated
10. 10
    其他to give 2.7 g

实验过程

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.

来源