Methanol → Methyl 3-methyl-6-(phenylthio)-benzoate

HRID 435663ノート

反応式

HRID 435663 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:8]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:23]O>>[CH3:1][C:2]1[CH:3]=[C:4]([C:8]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:9][CH:10]=1)[C:5]([O:7][CH3:23])=[O:6]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 125390985-Methyl-2-(phenylsulfanyl)benzoic acid

生成物 1

HCID 21481132Methyl 3-methyl-6-(phenylthio)-benzoate

実験手順

650 g of 3-methyl-6-(phenylthio)-benzoic acid in 7.5 litres of absolute methanol are slowly treated with 300 ml of concentrated sulphuric acid and the mixture is heated for 24 hours under reflux. The mixture is concentrated and the residue poured on to an ice-cold sodium bicarbonate solution. The mass is extracted with ether, washed with water, dried over sodium sulphate and concentrated. There is obtained methyl 3-methyl-6-(phenylthio)-benzoate as a red-brown oil which crystallises on standing.

後処理

  1. temperaturethe mixture is heated for 24 hours
  2. temperatureunder reflux
  3. concentrationThe mixture is concentrated
  4. additionthe residue poured on to an ice-cold sodium bicarbonate solution
  5. extractionThe mass is extracted with ether
  6. washwashed with water
  7. dry with materialdried over sodium sulphate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-98c136db2b6a4d2685aa1a7261988179
出典データセット
uspto-grants-1977_02
特許番号
US04006144

反応ノート

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