Hydrochloric Acid → ethyl 4-(3,4-dichlorophenyl)-2,4-dioxobutanoate

HRID 539650

反応式

HRID 539650 の反応式
CC([O-])(C)C.[K+].[CH3:7][C:8]([C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([Cl:17])[CH:11]=1)=[O:9].[CH2:18]([O:20][C:21](=[O:27])[C:22](OCC)=[O:23])[CH3:19].Cl>C1C=CC=CC=1>[Cl:17][C:12]1[CH:11]=[C:10]([C:8](=[O:9])[CH2:7][C:22](=[O:23])[C:21]([O:20][CH2:18][CH3:19])=[O:27])[CH:15]=[CH:14][C:13]=1[Cl:16]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 75841Ethanone, 1-(3,4-dichlorophenyl)-HCID 23665647Potassium tert-butoxide

生成物 1

HCID 10017017ethyl 4-(3,4-dichlorophenyl)-2,4-dioxobutanoate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To a solution of t-BuOK (0.05 mol, 5.6 g) in benzene (200 mL) was added dropwise a benzene (50 mL) solution of 3,4-dichloroacetophenone 5.1 (0.05 mol, 9.45 g) and diethyloxalate (0.055 mol, 8.1 g). The resultant mixture was stirred for 8 h at room temperature, then 10% aqueous HCl solution (100 mL) was added to the mixture. The organic layer was separated and washed with brine, dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography using dichloromethane as eluent to yield the title compound. Yield: 7.5 g (52%).

後処理

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by column chromatography

出典と根拠

ORDレコード
ord-1934ae3a8e0442dda759df426fd55823
出典データセット
uspto-grants-2014_10
特許番号
US08871761B2

関連ノート

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