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

HRID 374443
ノート
印刷プレビュー

反応式

HRID 374443 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒
HCID 962
Water
溶媒
HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cd034d164adc477c831d76eaf5b14afe
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05480894

反応ノート

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