Iodopentafluoroethane → HCID 178506327, 화합물

HRID 2243281

반응식

HRID 2243281 반응식
I[C:2]1[C:3]([C:7]([F:13])([F:12])[C:8]([F:11])([F:10])[F:9])=[N:4][NH:5][CH:6]=1.I[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17]>[Cu].CN(C=O)C>[F:12][C:7]([F:13])([C:3]1[C:2]([C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17])=[CH:6][NH:5][N:4]=1)[C:8]([F:11])([F:10])[F:9]

참가 물질

5

반응물 2

HCID 9636IodopentafluoroethaneHCID 178506332HCID 178506332, 화합물

생성물 1

HCID 178506327HCID 178506327, 화합물수율 9.9%

시약·촉매·용매 2

HCID 23978Copper촉매HCID 6228Dimethylformamide용매

반응 조건

온도
122.5 °C

실험 절차

4-Iodo-3-pentafluoroethyl-1H-pyrazole (12.48 g), copper powder (7.63 g), iodopentafluoroethane (29.50 g) and DMF (60 ml) were set in an autoclave and heated and stirred for 8 hours, maintaining the inside temperature of 120-125° C. After cooling to room temperature, the insoluble material was filtered off through Celite and washed with diethyl ether. The filtrate was diluted with water and extracted with diethyl ether. The organic phase was washed with water and dried over sodium sulfate, and concentrated under the reduced pressure. The crude product was distilled under reduced pressure to obtain 3,4-bis-pentafluoroethyl-1H-pyrazole (1.20 g), bp. 110-115° C./20 mbar.

후처리

  1. temperatureheated
  2. temperatureAfter cooling to room temperature
  3. filtrationthe insoluble material was filtered off through Celite
  4. washwashed with diethyl ether
  5. additionThe filtrate was diluted with water
  6. extractionextracted with diethyl ether
  7. washThe organic phase was washed with water
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated under the reduced pressure
  10. distillationThe crude product was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-e303a7e8bf0b4a68b5db9d22217ccab1
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674807B2

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