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

HRID 1741988
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HRID 1741988 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f42ceb4a8b6d4008b04b6fe30e438c13
출처 데이터셋
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05336482

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