Acetyl chloride → Methyl 3-acetyl-2-methylbenzofuran-7-carboxylate

HRID 1761934ノート

反応式

HRID 1761934 の反応式
[CH3:1][C:2]1[O:3][C:4]2[C:10]([C:11]([O:13][CH3:14])=[O:12])=[CH:9][CH:8]=[CH:7][C:5]=2[CH:6]=1.[C:15](Cl)(=[O:17])[CH3:16].[Cl-].[Al+3].[Cl-].[Cl-]>ClC(Cl)C>[C:15]([C:6]1[C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([C:11]([O:13][CH3:14])=[O:12])[C:4]=2[O:3][C:2]=1[CH3:1])(=[O:17])[CH3:16]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 14229729Methyl 2-methyl-1-benzofuran-7-carboxylate

生成物 1

HCID 14229733Methyl 3-acetyl-2-methylbenzofuran-7-carboxylate収率 88.5%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

A mixture of 1.0 g of methyl 2-methylbenzofuran-7-carboxylate, 1.24 g of acetyl chloride, 2.15 g of aluminum chloride and 20 ml of dichloroethane is heated at 50°-60° C. for 1 hour. The reaction mixture is poured into ice-water and the aqueous mixture is extracted with chloroform. The extract is washed with water, dried and evaporated to remove solvent. The residue is recrystallized from ethyl acetate-n-hexane to give 1.08 g of methyl 3-acetyl-2-methylbenzofuran-7-carboxylate as colorless needles.

後処理

  1. temperatureis heated at 50°-60° C. for 1 hour
  2. extractionthe aqueous mixture is extracted with chloroform
  3. washThe extract is washed with water
  4. customdried
  5. customevaporated
  6. customto remove solvent
  7. customThe residue is recrystallized from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-f6323838053e448f9fcde35dcc226a4c
出典データセット
uspto-grants-1989_05
特許番号
US04829067

反応ノート

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