Water → Methyl 1-methylpyrrole-2-carboxylate

HRID 127585

反応式

HRID 127585 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7]([OH:9])=[O:8].[H-].[Na+].O.[CH3:13]N(C)C=O>>[CH3:13][O:8][C:7]([C:3]1[N:2]([CH3:1])[CH:6]=[CH:5][CH:4]=1)=[O:9]

参加物

5

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 814531-Methyl-2-pyrrolecarboxylic acid

生成物 1

HCID 142178Methyl 1-methylpyrrole-2-carboxylate

実験手順

The starting material is prepared as follows: The solution of 28 g of 1-methylpyrrole-2-carboxylic acid in 20 ml of dimethylformamide is added to the suspension prepared from 12 g of 50% sodium hydride in mineral oil, washed with petroleum ether and suspended in 50 ml of dimethylformamide, while stirring and cooling. Thereupon 30 ml of methyl iodide are added and stirring is continued at ambient temperature. Another 10 ml of methyl iodide are added after the initial exothermic reaction has subsided. After standing overnight, the mixture is treated with water, extracted with diethyl ether, the extract washed with aqueous sodium carbonate and water, dried and evaporated, to yield the 1-methylpyrrole-2-carboxylic acid methyl ester as an oil.

後処理

  1. customThe starting material is prepared
  2. washwashed with petroleum ether
  3. temperaturecooling
  4. additionThereupon 30 ml of methyl iodide are added
  5. stirringstirring
  6. customis continued at ambient temperature
  7. additionAnother 10 ml of methyl iodide are added after the initial
  8. customexothermic reaction
  9. extractionextracted with diethyl ether
  10. washthe extract washed with aqueous sodium carbonate and water
  11. customdried
  12. customevaporated

出典と根拠

ORDレコード
ord-327e6677693244048f46825f908227e6
出典データセット
uspto-grants-1981_03
特許番号
US04256759

関連ノート

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