Iodopentafluoroethane → HCID 178506327、化合物

HRID 2243281ノート

反応式

HRID 2243281 の反応式
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]

参加物

5

反応物 2

HCID 9636IodopentafluoroethaneHCID 178506332HCID 178506332、化合物

生成物 1

HCID 178506327HCID 178506327、化合物収率 9.9%

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
122.5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e303a7e8bf0b4a68b5db9d22217ccab1
出典データセット
uspto-grants-2010_03
特許番号
US07674807B2

反応ノート

読み込み中…