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

HRID 1583366ノート

反応式

HRID 1583366 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

反応物 3

HCID 887MethanolHCID 24813Phosphorus oxychlorideHCID 31633966-Methyl-1H-indole-2-carboxylic acid

生成物 1

HCID 4715128methyl 6-methyl-1H-indole-2-carboxylate

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-d885f50433e44c1e87296268805ce8f0
出典データセット
uspto-grants-1985_11
特許番号
US04551468

反応ノート

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