Ethanol → HCID 21084111, 화합물

HRID 347828

반응식

HRID 347828 반응식
[Br:1][C:2]1[N:7]2[N:8]=[C:9]([CH2:14][CH3:15])[C:10]([N+:11]([O-])=O)=[C:6]2[CH:5]=[CH:4][CH:3]=1.C(O)C.O>[Zn].C(O)(=O)C>[Br:1][C:2]1[N:7]2[N:8]=[C:9]([CH2:14][CH3:15])[C:10]([NH2:11])=[C:6]2[CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 702EthanolHCID 962WaterHCID 219844817-Bromo-2-ethyl-3-nitropyrazolo[1,5-a]pyridine

생성물 1

HCID 21084111HCID 21084111, 화합물수율 73.3%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

반응 조건

온도
65 °C

실험 절차

To a suspension of 7-bromo-2-ethyl-3-nitropyrazolo[1,5-a]pyridine (1.78 g) in a mixed solution of ethanol (100 mL), water (50 mL) and acetic acid (10 mL) was added zinc powder (1.78 g) at room temperature and the reaction mixture was stirred for 1 hour at 65° C. The reaction mixture was filtered through celite to remove insoluble residue and the filtrate was evaporated under reduced pressure. Water was added to the obtained residue and extraction was performed with ethyl acetate, and after washing the organic extract with water, saturated aqueous sodium bicarbonate and brine, the organic extract was dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (60 g) and the title compound (1.16 g) was obtained as a dark green oil from the ethyl acetate:n-hexane (4:1) fraction.

후처리

  1. filtrationThe reaction mixture was filtered through celite
  2. customto remove insoluble residue
  3. customthe filtrate was evaporated under reduced pressure
  4. additionWater was added to the obtained residue and extraction
  5. washafter washing the
  6. extractionorganic extract with water, saturated aqueous sodium bicarbonate and brine
  7. extractionthe organic extract
  8. dry with materialwas dried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. customthe solvent was evaporated under reduced pressure
  11. customThe obtained residue was purified by silica gel column chromatography (60 g)

출처 및 근거

ORD 기록
ord-f7f28f656561437ea9b8e6ac9dac057a
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176216B2

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