반응 #1425

반응 방정식

Potassium bromide

D-norleucine

sodium nitrite

→

crude title product

(S)-2-Bromohexanoic acid

용매

sulfuric acid

반응 조건

후처리

1. 1
   온도maintaining the temperature between -10° and -5° C
2. 2
   workup.ADDITIONAfter addition
3. 3
   기타the foamy reaction
4. 4
   온도warmed to room temperature
5. 5
   workup.STIRRINGstirred for another hour
6. 6
   추출The reaction mixture was then extracted twice with ether
7. 7
   세척the ether extracts were washed once with water
8. 8
   건조dried (magnesium sulfate)
9. 9
   여과filtered
10. 10
    기타evaporated
11. 11
    기타to give 3.3 g

실험 절차

Potassium bromide (15.9 g., 133 mmol.) was added to a stirred solution of D-norleucine (5.0 g., 38 mmol.) in 2.5N sulfuric acid (77 ml.) at room temperature. The reaction mixture was cooled to -10° C. and solid sodium nitrite (3.94 g., 57 mmol.) was added portionwise, maintaining the temperature between -10° and -5° C. After addition was complete, the foamy 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 3.3 g. of crude title product.

출처