Potassium Hydroxide → HCID 21717332, 화합물

HRID 1386094노트

반응식

HRID 1386094 반응식
[OH-].[K+].[OH:3][C:4]1[C:5]([N+:11]([O-:13])=[O:12])=[N:6][CH:7]=[C:8]([CH3:10])[CH:9]=1.[K].[CH3:15][C:16]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:17]=1[CH2:18]Cl>C(O)C>[CH3:15][C:16]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:17]=1[CH2:18][O:3][C:4]1[C:5]([N+:11]([O-:13])=[O:12])=[N:6][CH:7]=[C:8]([CH3:10])[CH:9]=1

참가 물질

6

반응물 4

HCID 14797Potassium Hydroxide2회HCID 2211542,6-Dimethylbenzyl Chloride2회HCID 5462222PotassiumHCID 217660195-Methyl-2-nitropyridin-3-ol

생성물 1

HCID 21717332HCID 21717332, 화합물수율 81.1%

시약·촉매·용매 1

HCID 702Ethanol용매3회

실험 절차

To 0.52 g (8.02 mmol) of 87% KOH and 0.15 g q-iodide in 6 ml 95% ethanol was added a solution of 3-hydroxy-5-methyl-2-nitropyridine (1.2 g, 7.79 mmol) in 25 ml of ethanol. To the resulting suspension of the potassium salt was added dropwise a solution of 2,6-dimethyl benzylchloride (1.24 g, 8.02 mmol) in 13 ml of ethanol. The reaction mixture was refluxed for 1 h. More 87% KOH (0.16 g) and 2,6-dimethylbenzylchloride (0.38 g) were added. The reaction mixture was refluxed for additional 70 min. The mixture was filtered and the inorganic salts were washed with ethanol and methylene chloride. The organic layer was evaporated in vacuo. The residue was dissolved in methylene chloride, washed with aqueous NaHCO3, dried and evaporated in vacuo. The residue was suspended in ether/isopropanol and filtered to give 1.72 g (81%) of the title compound.

후처리

  1. temperatureThe reaction mixture was refluxed for 1 h
  2. temperatureThe reaction mixture was refluxed for additional 70 min
  3. filtrationThe mixture was filtered
  4. washthe inorganic salts were washed with ethanol and methylene chloride
  5. customThe organic layer was evaporated in vacuo
  6. dissolutionThe residue was dissolved in methylene chloride
  7. washwashed with aqueous NaHCO3
  8. customdried
  9. customevaporated in vacuo
  10. filtrationfiltered

출처 및 근거

ORD 기록
ord-75f2cc39dc7a474190888369be86b8ef
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265415B1

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