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3-(Dimethylamino)-2-[3-(trifluoromethyl)phenyl]prop-2-enal → 1-(2-Hydroxybutyl)-4-(m-trifluoromethylphenyl)-pyrazole

HRID 1973423
ノート
印刷プレビュー

反応式

HRID 1973423 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:4]=[C:5]([C:9](=[CH:12]N(C)C)[CH:10]=O)[CH:6]=[CH:7][CH:8]=1.[OH:18][CH:19]([CH2:23][CH3:24])[CH2:20][NH:21][NH2:22]>C1C=CC=CC=1>[OH:18][CH:19]([CH2:23][CH3:24])[CH2:20][N:21]1[CH:10]=[C:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:17])[F:16])[CH:4]=2)[CH:12]=[N:22]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 37090863-(Dimethylamino)-2-[3-(trifluoromethyl)phenyl]prop-2-enalHCID 41131272-Hydroxybutylhydrazine

生成物 1

HCID 214915151-(2-Hydroxybutyl)-4-(m-trifluoromethylphenyl)-pyrazole

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 10 g. of 2-(m-trifluoromethylphenyl)-3-dimethylaminoacrolein, 5 g. of 2-hydroxybutylhydrazine and 100 ml. of benzene is refluxed for 2.5 hours. The benzene is evaporated off, ether added, and the reaction mixture cooled to obtain a precipitate which is recovered by filtering, washed with pentane, dissolved in methylene chloride, dried, treated with charcoal and filtered. The resulting solution is treated by addition of pentane and the resulting precipitate recovered by filtering, washed with pentane and dried under reduced pressure to obtain 1-(2-hydroxybutyl)-4-(m-trifluoromethylphenyl)-pyrazole, m.p. 77°-79°C.

後処理

  1. additionA mixture of 10 g
  2. customThe benzene is evaporated off
  3. additionether added
  4. temperaturethe reaction mixture cooled
  5. customto obtain a precipitate which
  6. customis recovered
  7. filtrationby filtering
  8. washwashed with pentane
  9. dissolutiondissolved in methylene chloride
  10. customdried
  11. additiontreated with charcoal
  12. filtrationfiltered
  13. additionThe resulting solution is treated by addition of pentane
  14. customthe resulting precipitate recovered
  15. filtrationby filtering
  16. washwashed with pentane
  17. customdried under reduced pressure

出典と根拠

ORDレコード
ord-6993e45d70424c79aed0e971f28cdfc6
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03997555

反応ノート

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