4-Chloro-3-methylphenol → 1-Chloro-4-methoxy-2-methylbenzene

HRID 544335

反応式

HRID 544335 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[CH3:9].[C:10](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:10])=[CH:4][C:3]=1[CH3:9]

参加物

5

反応物 3

HCID 17324-Chloro-3-methylphenolHCID 6328Methyl iodideHCID 11430Potassium Carbonate

生成物 1

HCID 4581561-Chloro-4-methoxy-2-methylbenzene

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

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)].

後処理

  1. filtrationThe reaction mixture was filtered
  2. customthe filtrate evaporated to an oil
  3. additioncontaining solids
  4. customThe organic layer was separated
  5. washwashed in sequence with two portions of 1N sodium hydroxide, two portions of water and one portion of brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-289984adbf8d495fb4a0e22340a457c2
出典データセット
uspto-grants-1984_05
特許番号
US04448971

関連ノート

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