Nitric Acid → HCID 14835236, 화합물

HRID 1084903노트

반응식

HRID 1084903 반응식
[CH:1]([NH:3][CH:4]1[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5]1)=[O:2].[N+:13]([O-])([OH:15])=[O:14]>>[CH:1]([NH:3][CH:4]1[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N+:13]([O-:15])=[O:14])[CH:10]=2)[CH2:5]1)=[O:2]

참가 물질

3

반응물 2

HCID 944Nitric AcidHCID 14835235N-(2,3-Dihydro-1H-inden-2-yl)formamide

생성물 1

HCID 14835236HCID 14835236, 화합물

실험 절차

2-Formylaminoindane (15 g) was added portionwise to fuming nitric acid (30 ml, density=1.5 g/ml) whilst keeping the temperature at between 0° and -5°. Stirring was continued for 1 hour at 0° before pouring the reaction mixture onto ice/water and extracting with methylene chloride. The organic layer was washed with aqueous sodium bicarbonate, dried (MgSO4) and evaporated in vacuo to give an oil which was purified by column chromatography on silica eluting with methylene chloride containing hexane (20% down to 0%) and then methylene chloride containing methanol (0% up to 2%). The product-containing fractions were combined and evaporated to give the title compound, yield 7.7 g, m.p. 91°-92°.

후처리

  1. customat between 0° and -5°
  2. additionbefore pouring the reaction mixture onto ice/water
  3. extractionextracting with methylene chloride
  4. washThe organic layer was washed with aqueous sodium bicarbonate
  5. dry with materialdried (MgSO4)
  6. customevaporated in vacuo
  7. customto give an oil which
  8. customwas purified by column chromatography on silica eluting with methylene chloride
  9. additioncontaining hexane (20% down to 0%)
  10. additionmethylene chloride containing methanol (0% up to 2%)
  11. customevaporated

출처 및 근거

ORD 기록
ord-21b08dc909624e0fba376b4e870baa79
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05006561

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