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Methane → 3-Hydroxy-2-methyl-1-(propan-2-yl)pyridin-4(1H)-one

HRID 1741988
ノート
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反応式

HRID 1741988 の反応式
[OH:1][CH:2]1[C:7](=[O:8])[CH:6]=[CH:5][N:4]=[C:3]1[CH3:9].[CH:10](N)([CH3:12])[CH3:11].C>O.CC(C)=O>[CH:10]([N:4]1[CH:5]=[CH:6][C:7](=[O:8])[C:2]([OH:1])=[C:3]1[CH3:9])([CH3:12])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 297MethaneHCID 6363IsopropylamineHCID 666058152-Methyl-3-hydroxy-4-pyridone

生成物 1

HCID 101301403-Hydroxy-2-methyl-1-(propan-2-yl)pyridin-4(1H)-one

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

1-Isopropyl-3-hydroxy-2-methylpyrid-4-one was prepared by refluxing 3-hydroxy-2-methylpyrid-4-one (Maltol) (10.0 g) with 3 equivalents of isopropylamine (99%) in 200 ml of water for 8 hours. Decolorizing charcoal was added after refluxing and the mixture was stirred for 0.5 hours. The mixture was then filtered through a medium frit filter containing 0.5 inches of Celite. The filtered solution was then concentrated in vacuo (rotary evaporator) to remove the water and excess amine, leaving a dark thick oil. The oil was then dissolved in minimal amounts of hot acetone and filtered (repeatedly) through a medium frit filter. Brownish crystals (product) remained on the frit and these were then washed (3X) with 1 ml portions of hot acetone to obtain white crystals. m.p. 239°-242 ° C.

後処理

  1. temperatureafter refluxing
  2. filtrationThe mixture was then filtered through a medium frit
  3. filtrationfilter
  4. additioncontaining 0.5 inches of Celite
  5. concentrationThe filtered solution was then concentrated in vacuo (rotary evaporator)
  6. customto remove the water and excess amine
  7. customleaving a dark thick oil
  8. filtrationfiltered (repeatedly) through a medium frit
  9. filtrationfilter
  10. washthese were then washed (3X) with 1 ml portions of hot acetone
  11. customto obtain white crystals

出典と根拠

ORDレコード
ord-f42ceb4a8b6d4008b04b6fe30e438c13
出典データセット
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05336482

反応ノート

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