Acetic Anhydride → HCID 178471869、化合物

HRID 47891ノート

反応式

HRID 47891 の反応式
[C:1]([C:3]1[C:4]([Cl:19])=[C:5]([CH:14]=[C:15]([F:18])[C:16]=1[Cl:17])[C:6]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7])#[N:2].[CH:20](OCC)(OCC)OCC.C(OC(=O)C)(=O)C.[CH:37]1([NH2:40])[CH2:39][CH2:38]1>>[C:1]([C:3]1[C:4]([Cl:19])=[C:5]([CH:14]=[C:15]([F:18])[C:16]=1[Cl:17])[C:6]([C:8](=[CH:20][NH:40][CH:37]1[CH2:39][CH2:38]1)[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7])#[N:2]

参加物

5

反応物 4

HCID 7918Acetic AnhydrideHCID 31214Ethyl orthoformateHCID 69828CyclopropylamineHCID 86589175Ethyl 3-cyano-2,4-dichloro-5-fluorobenzoylacetate

生成物 1

HCID 178471869HCID 178471869、化合物収率 70.1%

実験手順

76.0 g of ethyl 3-cyano-2,4-dichloro-5-fluorobenzoylacetate (0.25 mol), 66.6 g of triethyl orthoformate (0.45 mol) and 77.4 g of diacetyl oxide (0.72 mol) were stirred at 150° C. for 2.5 hours. Fractions having a lower boiling point were evaporated under reduced pressure. To the residue was added 250 ml of anhydrous ethanol. 14.5 g of cyclopropylamine (0.25 mol) was added to the solution and the reaction was then carried out for 2 hours. The resulting mixture was filtered under suction. The residue was recrystallized from a mixture of petroleum ether and cyclohexane to yield 65.0 g (0.175 mol) of ethyl 2-(3-cyano-2,4-dichloro-5-fluorobenzoyl)-3-cyclopropylaminoacrylate in 70.1% yield.

後処理

  1. customwere evaporated under reduced pressure
  2. additionTo the residue was added 250 ml of anhydrous ethanol
  3. filtrationThe resulting mixture was filtered under suction
  4. customThe residue was recrystallized from a mixture of petroleum ether and cyclohexane

出典と根拠

ORDレコード
ord-670782c6bd174e549333fde5e909bd54
出典データセット
uspto-grants-2004_03
特許番号
US06699992B2

反応ノート

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