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Potassium Carbonate → Ethyl 3,4,5-tribromo-alpha-butylpyrazole-1-acetate

HRID 372195
ノート
印刷プレビュー

反応式

HRID 372195 の反応式
[Br:1][C:2]1[C:6]([Br:7])=[C:5]([Br:8])[NH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:16]([CH2:22][CH2:23][CH2:24][CH3:25])[C:17]([O:19][CH2:20][CH3:21])=[O:18]>CC(C)=O>[Br:1][C:2]1[C:6]([Br:7])=[C:5]([Br:8])[N:4]([CH:16]([CH2:22][CH2:23][CH2:24][CH3:25])[C:17]([O:19][CH2:20][CH3:21])=[O:18])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 79072Ethyl 2-bromohexanoateHCID 6276743,4,5-tribromo-1H-pyrazole

生成物 1

HCID 20328047Ethyl 3,4,5-tribromo-alpha-butylpyrazole-1-acetate収率 92%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A quantity (30.4 g., 0.1 mole) of 3,4,5-tribromopyrazole was dissolved in 500 ml. acetone and 27.6 g. (0.2 mole) solid anhydrous potassium carbonate was added. The mixture was heated at the reflux temperature with stirring for 10 minutes and after cooling 23.0 g. (0.11 mole) ethyl 2-bromohexanoate was added. This reaction mixture was heated at the reflux temperature for 11/2 hrs., cooled, and then filtered. The solids on the filter were washed with acetone and the combined acetone filtrate and acetone washes were evaporated to dryness under reduced pressure. Distillation of the residue yielded ethyl 3,4,5-tribromo-α-butylpyrazole-1-acetate, 41.0 g. (92% yield), having a boiling point at 138° to 140° C. at 0.15 mm. mercury pressure.

後処理

  1. temperatureThe mixture was heated at the reflux temperature
  2. temperatureafter cooling 23.0 g
  3. temperatureThis reaction mixture was heated at the reflux temperature for 11/2 hrs
  4. temperature, cooled
  5. filtrationfiltered
  6. washThe solids on the filter were washed with acetone
  7. customthe combined acetone filtrate and acetone washes were evaporated to dryness under reduced pressure
  8. distillationDistillation of the residue

出典と根拠

ORDレコード
ord-7428e029225e48c886eb12fe5c40d1a3
出典データセット
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04089672

反応ノート

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