反応 #631517

ord-289984adbf8d495fb4a0e22340a457c2

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The reaction mixture was filtered
  2. 2
    その他the filtrate evaporated to an oil
  3. 3
    workup.ADDITIONcontaining solids
  4. 4
    その他The organic layer was separated
  5. 5
    洗浄washed in sequence with two portions of 1N sodium hydroxide, two portions of water and one portion of brine
  6. 6
    乾燥dried over anhydrous magnesium sulfate
  7. 7
    濃縮concentrated

実験手順

4-Chloro-3-methylphenol (28.5 g., 0.2 mole) was dissolved in 400 ml. of acetone. Potassium carbonate (33.1 g., 0.24 mole) and then methyl iodide (34.1 g., 0.24 mole) were added and the mixture stirred for 16 hours at room temperature. The reaction mixture was filtered and the filtrate evaporated to an oil containing solids. This residue was distributed between methylene chloride and water. The organic layer was separated, washed in sequence with two portions of 1N sodium hydroxide, two portions of water and one portion of brine, dried over anhydrous magnesium sulfate and concentrated to yield 4-chloro-3-methylanisole as an oil [24.6 g., 86%, pnmr/CDCl3 /delta. 2.3 (s, 3H), 3.7 (s, 3H) 6.9 (m, 3H)].

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04448971uspto-grants-1984_05