반응 #2358542

반응 방정식

m-Chloroperbenzoic acid

N-(cyclohex-3-en-1(R)-yl)-2,2,2-trifluoro-acetamide

N-(Cyclohex-3-en-1(R)-yl)-2,2,2-trifluoro-acetamide

→

mCBA

반응 조건

후처리

1. 1
   workup.ADDITIONcontaining the
2. 2
   세척rinsed through with 69.5 ml of chlorobenzene
3. 3
   기타The mixture obtained
4. 4
   기타Upon completion of the reaction
5. 5
   기타the mixture obtained
6. 6
   온도was cooled to 0 to −5° C.
7. 7
   workup.STIRRINGstirred for 30 min

실험 절차

106.5 g of m-Chloroperbenzoic acid (70%) was charged portionwise to the vessel containing the cooled (10-15° C.) solution of 69.5 g of the N-(cyclohex-3-en-1(R)-yl)-2,2,2-trifluoro-acetamide of step A maintaining temperature <30° C., and rinsed through with 69.5 ml of chlorobenzene. The mixture obtained was stirred at 20 to 25° C. for 1 h and the reaction was followed by TLC until completion. Upon completion of the reaction, the mixture obtained was cooled to 0 to −5° C., stirred for 30 min and the solid precipitate (mCBA) obtained was filtered off and washed with 2×34.8 ml of chlorobenzene. The resultant filtrate was washed with 347.6 ml of 10% sodium thiosulfate solution to remove peroxides, and the resultant aqueous layer was back extracted with 208.6 ml of chlorobenzene. The combined organic layers obtained were washed with 347.6 ml of 5% sodium bicarbonate solution to ensure a pH>7 of the aqueous phase and the resultant aqueous layer was back extracted with 208.6 ml of chlorobenzene. The combined organic layers were washed with 347.6 ml of water.

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