Benzyl Bromide → Ethyl alpha-benzylacetoacetate

HRID 898497

反応式

HRID 898497 の反応式
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].C([O-])([O-])=O.[K+].[K+].[CH2:16](Br)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[NH4+].[Cl-]>C1C=CC=CC=1>[CH2:16]([CH:2]([C:3](=[O:4])[CH3:5])[C:1]([O:7][CH2:8][CH3:9])=[O:6])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

6

反応物 4

HCID 7498Benzyl BromideHCID 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 25517Ammonium Chloride

生成物 1

HCID 246929Ethyl alpha-benzylacetoacetate収率 74%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

0.1 Mol of ethyl acetoacetate, 0.1 mol of K2CO3, 0.1 mol of benzyl bromide, 0.01 mmol of PEG-400 (polyethylene glycol 400) and 100 ml of benzene were stirred at 75° C. for 7 hours. After cooling, 20 ml of saturated solution of NH4Cl was added to dissolve solid, and product was extracted with ethyl acetate. After removing the solvent, the residue was distilled under reduced pressure, and a cut fraction was collected at 116-118° C./20 Pa. Yield 74%.

後処理

  1. temperatureAfter cooling
  2. dissolutionto dissolve solid, and product
  3. extractionwas extracted with ethyl acetate
  4. customAfter removing the solvent
  5. distillationthe residue was distilled under reduced pressure
  6. customa cut fraction was collected at 116-118° C./20 Pa

出典と根拠

ORDレコード
ord-e2405c4aecdd42af8025950385979ec4
出典データセット
uspto-grants-2008_04
特許番号
US07351778B2

関連ノート

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