Potassium Carbonate → Butyl-a-bromoacrylate

HRID 1648976

反応式

HRID 1648976 の反応式
[Br:1][CH:2]([CH2:10]Br)[C:3]([O:5][CH2:6][CH2:7][CH2:8][CH3:9])=[O:4].C(=O)([O-])[O-].[K+].[K+]>COC1C=CC(O)=CC=1.C(#N)C>[Br:1][C:2](=[CH2:10])[C:3]([O:5][CH2:6][CH2:7][CH2:8][CH3:9])=[O:4]

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 519844Propanoic acid, 2,3-dibromo-, butyl ester

生成物 1

HCID 19901948Butyl-a-bromoacrylate収率 90.9%

試薬・触媒・溶媒 2

HCID 90154-Methoxyphenol触媒HCID 6342Acetonitrile溶媒

実験手順

The product (300 g) of Step 1 and p-methoxyphenol (2 g) was added to a 2 l. round bottom flask fitted with a thermometer, condenser, stirrer and inlet for nitrogen, and containing acetonitrile (1000 ml) and anhydrous potassium carbonate (330 g). The reaction mixture was stirred under reflux for 8 hours and cooled, and the salts were filtered off. The filtrate was evaporated under reduced pressure to remove the solvent, and the residue was dissolved in dichloromethane. The solution was dried (Na2SO4), filtered and evaporated. Distillation of the residue afforded n-butyl 2-bromoacrylate (196 g; 90%), b.p. 90°/15 mmHg.

後処理

  1. customround bottom flask fitted with a thermometer, condenser, stirrer and inlet for nitrogen
  2. temperatureunder reflux for 8 hours
  3. temperaturecooled
  4. filtrationthe salts were filtered off
  5. customThe filtrate was evaporated under reduced pressure
  6. customto remove the solvent
  7. dissolutionthe residue was dissolved in dichloromethane
  8. dry with materialThe solution was dried (Na2SO4)
  9. filtrationfiltered
  10. customevaporated
  11. distillationDistillation of the residue

出典と根拠

ORDレコード
ord-1b01719e826d4861abd8b95da613c813
出典データセット
uspto-grants-1983_11
特許番号
US04414391

関連ノート

読み込み中…