Formic Acid → Methyl 5-acetyl-2-chlorobenzoate

HRID 1988370ノート

反応式

HRID 1988370 の反応式
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([C:10]#[C:11][Si](C)(C)C)[CH:7]=[CH:6][C:5]=1[Cl:16].C(O)=[O:19]>>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([C:10](=[O:19])[CH3:11])[CH:7]=[CH:6][C:5]=1[Cl:16]

参加物

3

反応物 2

HCID 284Formic AcidHCID 57422929Methyl 2-chloro-5-((trimethylsilyl)ethynyl)benzoate

生成物 1

HCID 58818179Methyl 5-acetyl-2-chlorobenzoate

実験手順

A mixture of 2-chloro-5-trimethylsilanylethynyl-benzoic acid methyl ester (3.2 g, 12 mmol) in formic acid (50 mL) was heated at reflux for 16 h. The mixture was cooled to room temperature and concentrated in vacuo. The residue was diluted with ethyl acetate and washed with saturated aqueous sodium bicarbonate, water and brine. The organic layer was dried, filtered and concentrated in vacuo to afford the title compound (1.4 g).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. concentrationconcentrated in vacuo
  4. additionThe residue was diluted with ethyl acetate
  5. washwashed with saturated aqueous sodium bicarbonate, water and brine
  6. customThe organic layer was dried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-789701d6c18149ef86b630ebdc7c5d1e
出典データセット
uspto-grants-2009_06
特許番号
US07553972B2

反応ノート

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