Water → Methyl 1-methylpyrrole-2-carboxylate

HRID 127585

반응식

HRID 127585 반응식
[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]

참가 물질

5

반응물 4

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

생성물 1

HCID 142178Methyl 1-methylpyrrole-2-carboxylate

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-327e6677693244048f46825f908227e6
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256759

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