Hydrochloric Acid → 4-Pyridinone,3-OH-2-Me

HRID 566863노트

반응식

HRID 566863 반응식
[CH3:1][C:2]1[NH:3][CH:4]=[CH:5][C:6](=[O:16])[C:7]=1[O:8]CC1C=CC=CC=1.Cl>[Pd].C(O)C>[CH3:1][C:2]1[NH:3][CH:4]=[CH:5][C:6](=[O:16])[C:7]=1[OH:8]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 27264163-(Benzyloxy)-2-methylpyridin-4(1H)-one

생성물 1

HCID 3238144-Pyridinone,3-OH-2-Me수율 67.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

1.00 g (2.68 mmol) of 2-methyl-3-benzyloxypyridine-4(1H)-one of dimethylene xylitol compound is put into a mixture of 10 mL ethanol—2 mL H2O; then 0.08 g of Pd/C at 10% is added, and the pH of the solution is adjusted to pH=1 with a solution of concentrated HCl. The reaction medium is then subjected to catalytic hydrogenolysis under agitation at room temperature for 4 hours. At the end of this hydrogenolysis, the reaction medium is filtered. Then, 25 mL of water is added to the residue, and the solution is neutralized by addition of an aqueous solution of soda. The reaction medium is extracted with 2×20 mL of dichloromethane; the organic phases are collected, dried on sodium sulphate, filtered, and evaporated under reduced pressure; 509 mg (1.80 mmol) of 2-methyl-3-hydroxypyridine-4(1H)-one of dimethylene xylitol is isolated, which is pure at chromatographic and NMR analyses. Yield: 67%.

후처리

  1. filtrationAt the end of this hydrogenolysis, the reaction medium is filtered
  2. additionThen, 25 mL of water is added to the residue
  3. additionthe solution is neutralized by addition of an aqueous solution of soda
  4. extractionThe reaction medium is extracted with 2×20 mL of dichloromethane
  5. customthe organic phases are collected
  6. customdried on sodium sulphate
  7. filtrationfiltered
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-a03787d4a018453aa650efd075cc6330
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06177409B1

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