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

HRID 1973423
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반응식

HRID 1973423 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6993e45d70424c79aed0e971f28cdfc6
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03997555

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