Potassium Carbonate → Butyl-a-bromoacrylate

HRID 1648976

반응식

HRID 1648976 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 19901948Butyl-a-bromoacrylate수율 90.9%

시약·촉매·용매 2

HCID 90154-Methoxyphenol촉매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1b01719e826d4861abd8b95da613c813
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04414391

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