Water → Methyl 3-chloro-p-anisate

HRID 1283640

反応式

HRID 1283640 の反応式
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([Cl:11])[CH:5]=1.[OH-].[Na+].O.S(OC)(O[CH3:20])(=O)=O>CCOCC>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:20])=[C:6]([Cl:11])[CH:5]=1

参加物

6

実験手順

To a cooled solution of 14.5 g. (0.078 mol.) of 3-chloro-4-hydroxybenzoic acid methyl ester and 4.0 g. (0.1 mol.) of sodium hydroxide in 100 ml. of water was dropwise added 9.8 g. (7.3 ml., 0.079 mol.) of dimethyl sulfate. The reaction mixture was refluxed for two hours. After cooling, ether was added and the layers were separated. The organic phase was washed with water, dilute sulfuric acid and water, dried (Na2SO4) and concentrated in vacuo to give 3-chloro-4-methoxybenzoic acid methyl ester, m.p. 72°-74°.

後処理

  1. temperatureThe reaction mixture was refluxed for two hours
  2. temperatureAfter cooling
  3. customthe layers were separated
  4. washThe organic phase was washed with water, dilute sulfuric acid and water
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e844daecefa24991bf40461d7faffdea
出典データセット
uspto-grants-1976_08
特許番号
US03975537

関連ノート

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