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Hydrochloric Acid → 3-Benzyloxy-1-(2-hydroxyethyl)-2-methylpyridin-4-one

HRID 374443
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HRID 374443 반응식
[CH2:1]([O:8][C:9]1[C:14](=[O:15])[CH:13]=[CH:12]O[C:10]=1[CH3:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].[CH2:19]([CH2:21][NH2:22])[OH:20].Cl>C(O)C.C(OCC)C.O>[CH2:1]([O:8][C:9]1[C:14](=[O:15])[CH:13]=[CH:12][N:22]([CH2:21][CH2:19][OH:20])[C:10]=1[CH3:16])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 700EthanolamineHCID 14798Sodium HydroxideHCID 14901193-Benzyloxy-2-methyl-4-pyrone

생성물 1

HCID 4046803-Benzyloxy-1-(2-hydroxyethyl)-2-methylpyridin-4-one수율 44.94%

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 962
Water
용매
HCID 3283Diethyl Ether용매

실험 절차

A solution of the product from (1) in ethanol:water (300 ml:300 ml) containing 5% aqueous sodium hydroxide (2 ml) was treated with ethanolamine (17 ml) and then refluxed for 18 hours with rapid stirring. The resultant solution was cooled and adjusted to pH 1 with concentrated hydrochloric acid. The solid which formed on cooling was extracted with hot absolute ethanol and the precipitate obtained on cooling was taken up in diethylether, the solution being filtered and evaporated to dryness by rotary evaporation to give the title compound in 44.94% yield, m.p. 191.5°-193° C.

후처리

  1. temperaturerefluxed for 18 hours with rapid stirring
  2. customThe solid which formed
  3. temperatureon cooling
  4. extractionwas extracted with hot absolute ethanol
  5. customthe precipitate obtained
  6. temperatureon cooling
  7. filtrationthe solution being filtered
  8. customevaporated to dryness by rotary evaporation

출처 및 근거

ORD 기록
ord-cd034d164adc477c831d76eaf5b14afe
출처 데이터셋
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05480894

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