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Ethanol → Ethyl 5-methylimidazo[1,2-a]pyridine-3-carboxylate

HRID 1068824
ノート
印刷プレビュー

反応式

HRID 1068824 の反応式
[K].Cl[CH:3]([CH:9]=O)[C:4]([O:6][CH2:7][CH3:8])=[O:5].[NH2:11][C:12]1[N:17]=[C:16]([CH3:18])[CH:15]=[CH:14][CH:13]=1.C(O)C>C(O)(=O)C>[C:4]([C:3]1[N:17]2[C:16]([CH3:18])=[CH:15][CH:14]=[CH:13][C:12]2=[N:11][CH:9]=1)([O:6][CH2:7][CH3:8])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 157652-Amino-6-methylpyridineHCID 86623935Ethyl 2-chloro-3-oxopropanoate potassium salt

生成物 1

HCID 11816548Ethyl 5-methylimidazo[1,2-a]pyridine-3-carboxylate収率 57.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

In 10 ml of ether was suspended 560 mg (5.0 mM) of potassium tert-butoxide and while the suspension was vigorously stirred, a solution of ethyl formate:370 mg (5.00 mM) and ethyl chloroformate: 613 mg (5.00 mM) in 10 ml of ether was added dropwise over 3 minutes at room temperature. This mixture was stirred at room temperature for 30 minutes and the precipitate that formed was recovered by filtration and rinsed with a small amount of ether. This precipitate was dried in vacuo to give 700 mg (yield 73.8%) of ethyl 2-chloro-2-formylacetate potassium salt as light-yellow solid. Then, 700 mg (3.69 mM) of ethyl 2-chloro-2-formylacetate potassium salt and 399 mg (3.69 mM) of 6-amino-2-methylpyridine were mixed with 20 ml of ethanol and after addition of 0.53 ml (9.23 mM) of acetic acid, the whole mixture was refluxed for 3 hours. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was diluted with 20 ml of ethyl acetate and 20 ml of purified water. Then, saturated aqueous NaHCO3 solution was added until the water layer became pH 8. This mixture was extracted with 40 ml of ethyl acetate and the organic layer was washed with 30 ml of saturated aqueous NaCl solution and dried over MgSO4. The solvent was then distilled off under reduced pressure and the residue was purified by silica gel column chromatography (eluent: ethyl acetate) to provide 430 mg (yield 57.1%) of the title compound as light-yellow liquid.

後処理

  1. temperaturethe whole mixture was refluxed for 3 hours
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionthe residue was diluted with 20 ml of ethyl acetate and 20 ml of purified water
  5. additionThen, saturated aqueous NaHCO3 solution was added until the water layer
  6. extractionThis mixture was extracted with 40 ml of ethyl acetate
  7. washthe organic layer was washed with 30 ml of saturated aqueous NaCl solution
  8. dry with materialdried over MgSO4
  9. distillationThe solvent was then distilled off under reduced pressure
  10. customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate)

出典と根拠

ORDレコード
ord-9332848c3a844b8d907e00ce31c65050
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06251905B1

反応ノート

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