반응 #722157

반응 방정식

acetaldoxime

3-aminobenzotrifluoride

hydrochloric acid

sodium nitrite

→

3-trifluoromethylacetophenone

수율 51.8%

용매

water

water

water

반응 조건

후처리

1. 1
   기타At below −5° C.
2. 2
   기타metered in at below 0° C. over the course of 2 hours
3. 3
   온도was heated to 28° C.
4. 4
   workup.STIRRINGwith intensive stirring over the course of 2 hours
5. 5
   기타to react at 30° C. for another 30 minutes
6. 6
   workup.WAITAfter 1 hour
7. 7
   온도the mixture was heated to 100° C.
8. 8
   workup.DISTILLATIONthe crude product was distilled off together with water
9. 9
   기타After the removal of the water from the distillate
10. 10
    workup.DISTILLATIONthe crude product was distilled over a column

실험 절차

Under nitrogen, 1290 g of water and 740 g of hydrochloric acid (30% by weight strength) were initially charged and cooled to from −10 to −5° C. At below −5° C., 334 g of 3-aminobenzotrifluoride were then metered in (content 99.9%). 149 g of sodium nitrite were dissolved in 690 g of water and metered in at below 0° C. over the course of 2 hours. The mixture was then stirred for another 1 hour. Under nitrogen, an initial charge of 24 g of copper sulphate hydrate, 73 g of water and 183 g of acetaldoxime was heated to 28° C., and the diazonium salt solution which had been prepared beforehand was metered in with intensive stirring over the course of 2 hours. The mixture was allowed to react at 30° C. for another 30 minutes. After 1 hour, the mixture was heated to 100° C. and the crude product was distilled off together with water. After the removal of the water from the distillate, the crude product was distilled over a column. 202 g of 3-trifluoromethylacetophenone were obtained (content according to GC 99.1%). This corresponds to a yield of 51.5% of theory.

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