Methyl iodide → Methyl (4-fluorophenyl)methoxyacetate

HRID 1009399

反応式

HRID 1009399 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].[F:7][C:8]1[CH:18]=[CH:17][C:11]([CH:12]([OH:16])C(O)=O)=[CH:10][CH:9]=1.CI.[C:21]([O:24][CH2:25]C)(=[O:23])[CH3:22]>CN(C=O)C.O>[F:7][C:8]1[CH:9]=[CH:10][C:11]([CH2:12][O:16][CH2:22][C:21]([O:24][CH3:25])=[O:23])=[CH:17][CH:18]=1

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 10796Cesium carbonateHCID 980684-Fluoromandelic acid

生成物 1

HCID 57267346Methyl (4-fluorophenyl)methoxyacetate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Cesium carbonate (6.5 g) was added to a solution of 4-fluoromandelic acid (CAS #395-33-5, 1.7 g) and methyl iodide (1.9 mL) in DMF (15 ml), and the reaction solution was stirred at room temperature for 11 hours. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system) to obtain 1.22 g of the title compound. The property values of the compound are as follows.

後処理

  1. customthe organic layer was separated
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system)

出典と根拠

ORDレコード
ord-402944f252fe46458ff56e44e6e46225
出典データセット
uspto-grants-2011_07
特許番号
US07973033B2

関連ノート

読み込み中…