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

HRID 580261ノート

反応式

HRID 580261 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1d1d2e107bcd4aa8bc568ea5c96b3a86
出典データセット
uspto-grants-1988_06
特許番号
US04752326

反応ノート

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