Allyl bromide → 1-(2-Fluoro-4-chloro-5-allyloxyphenyl)-3,4,5-trimethylpyrazole

HRID 580261노트

반응식

HRID 580261 반응식
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N:10]1[C:14]([CH3:15])=[C:13]([CH3:16])[C:12]([CH3:17])=[N:11]1.[CH2:18](Br)[CH:19]=[CH2:20].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH2:20][CH:19]=[CH2:18])=[CH:4][C:3]=1[N:10]1[C:14]([CH3:15])=[C:13]([CH3:16])[C:12]([CH3:17])=[N:11]1

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 137982331-(2-Fluoro-4-chloro-5-hydroxyphenyl)-3,4,5-trimethylpyrazole

생성물 1

HCID 137982731-(2-Fluoro-4-chloro-5-allyloxyphenyl)-3,4,5-trimethylpyrazole수율 97.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 1-(2-fluoro-4-chloro-5-hydroxyphenyl)-3,4,5-trimethylpyrazole (25.5 g), allyl bromide (13.3 g), anhydrous potassium carbonate (14.5 g) and acetonitrile (150 ml) was heated under reflux, with stirring for 3 hours. After cooling, the reaction mixture was filtered through a filter to remove the inorganic salts therefrom and the filtrate was concentrated to a small volume under reduced pressure, affording the titled compound (28.7 g) as a pale brown crystalline solid. Recrystallization of this solid from cyclohexane yielded a white crystalline solid. m.p. 97°-99° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux
  3. temperatureAfter cooling
  4. filtrationthe reaction mixture was filtered through
  5. filtrationa filter
  6. customto remove the inorganic salts
  7. concentrationthe filtrate was concentrated to a small volume under reduced pressure

출처 및 근거

ORD 기록
ord-1d1d2e107bcd4aa8bc568ea5c96b3a86
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752326

반응 노트

불러오는 중…