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Acetone → HCID 21536645、化合物

HRID 1076445
ノート
印刷プレビュー

反応式

HRID 1076445 の反応式
[Br:1][C:2]1[C:3]([CH3:8])=[N:4][NH:5][C:6]=1[Br:7].CC(C)=O.C(=O)([O-])[O-].[K+].[K+].Br[CH:20]([CH3:26])[C:21]([O:23][CH2:24][CH3:25])=[O:22]>CCCCCC>[Br:7][C:6]1[C:2]([Br:1])=[C:3]([CH3:8])[N:4]([CH:20]([CH3:26])[C:21]([O:23][CH2:24][CH3:25])=[O:22])[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 180AcetoneHCID 11430Potassium CarbonateHCID 79040Ethyl 2-bromopropionateHCID 178434484HCID 178434484、化合物

生成物 1

HCID 21536645HCID 21536645、化合物収率 75%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

A reaction mixture consisting of a solution of 13.7 g. (0.057 mole) 4,5 -dibromo-3-methylpyrazole in 200 ml. acetone and 15.7 g. (0.114 mole) anhydrous potassium carbonate was heated at the reflux temperature with continuous stirring for 15 minutes. After cooling, 10.4 g. (0.06 mole) ethyl 2-bromopropionate was added. This reaction mixture was then heated at the reflux temperature for 2.5 hours. It was cooled and filtered. The acetone was then removed by evaporation under reduced pressure, and the residue thus obtained was dissolved in hot hexane. After chilling in a refrigerator the crystals that had formed were collected on a filter. There was thus obtained 14.5 g. (75% yield) of ethyl 3,4 -dibromo-α, 5-dimethylpyrazole-1-acetate having a melting point at 61° to 62° C.

後処理

  1. temperatureAfter cooling
  2. temperatureThis reaction mixture was then heated at the reflux temperature for 2.5 hours
  3. temperatureIt was cooled
  4. filtrationfiltered
  5. customThe acetone was then removed by evaporation under reduced pressure
  6. customthe residue thus obtained
  7. temperatureAfter chilling in a refrigerator the crystals that
  8. customhad formed
  9. customwere collected on a filter

出典と根拠

ORDレコード
ord-d61ce0befc9348c9aa69e373cc1211b2
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03957480

反応ノート

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