Hydrochloric Acid → 3-Pyridineacrylic acid ethyl ester

HRID 1492009

反応式

HRID 1492009 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[CH:8][C:9]([OH:11])=[O:10])[CH:2]=1.Cl.[CH2:13](O)[CH3:14]>>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[CH:8][C:9]([O:11][CH2:13][CH3:14])=[O:10])[CH:2]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 1019843-(3-Pyridinyl)-2-propenoic acid

生成物 1

HCID 5833373-Pyridineacrylic acid ethyl ester

実験手順

To a stirred suspension of 150 g of β-(3-pyridyl)acrylic acid in 1500 ml of ethanol a slow stream of hydrogen chloride gas is bubbled for 4 to 5 hr, where all solids dissolved. Approximately 500 ml of ethanol are distilled off at atmospheric pressure, the residual solution is cooled and diluted with 1500 ml of ether with stirring. The solids are filtered, washed with ether and resuspended in ethyl acetate. The stirred suspension is neutralized with conc. aq. sodium bicarbonate. The ethyl acetate layer is separated and the aqueous layer is extracted once more with ethyl acetate. The combined organic extracts are washed with brine, dried (MgSO4), evaporated and the residual oil is distilled to give 110 g of ethyl β-(3-pyridyl)acrylate with bp 95°-100° C., 0.1 mm/Hg.

後処理

  1. customis bubbled for 4 to 5 hr
  2. dissolutionwhere all solids dissolved
  3. distillationApproximately 500 ml of ethanol are distilled off at atmospheric pressure
  4. temperaturethe residual solution is cooled
  5. additiondiluted with 1500 ml of ether
  6. filtrationThe solids are filtered
  7. washwashed with ether
  8. customThe ethyl acetate layer is separated
  9. extractionthe aqueous layer is extracted once more with ethyl acetate
  10. washThe combined organic extracts are washed with brine
  11. dry with materialdried (MgSO4)
  12. customevaporated
  13. distillationthe residual oil is distilled

出典と根拠

ORDレコード
ord-f5c6fe08862f4615be16ca1d29f9b308
出典データセット
uspto-grants-1994_12
特許番号
US05371096

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