Methanol → methyl 6-methyl-1H-indole-2-carboxylate

HRID 648045ノート

反応式

HRID 648045 の反応式
[CH3:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[C:7]([C:11]([OH:13])=[O:12])[NH:8]2)=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)=O.[CH3:19]O>>[CH3:19][O:12][C:11]([C:7]1[NH:8][C:9]2[C:5]([CH:6]=1)=[CH:4][CH:3]=[C:2]([CH3:1])[CH:10]=2)=[O:13]

参加物

4

実験手順

A solution of 6-methylindole-2-carboxylic acid (38.2 g.) in methanol (400 ml.) containing phosphorus oxychloride (5 ml.) was heated under reflux for 4 hours and then evaporated. The residue was dissolved in chloroform and the solution was washed successively with water and sodium bicarbonate solution and then dried (Na2SO4). Evaporation of the solvent gave a solid which was crystallized from methanol to give 6-methylindole-2-carboxylic acid methyl ester (28.1 g.), m.p. 128°-131° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. customevaporated
  4. dissolutionThe residue was dissolved in chloroform
  5. washthe solution was washed successively with water and sodium bicarbonate solution
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of the solvent
  8. customgave a solid which
  9. customwas crystallized from methanol

出典と根拠

ORDレコード
ord-6ac1321ca2ad4af2af5ee61526032892
出典データセット
uspto-grants-1983_10
特許番号
US04410539

反応ノート

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