Nitric Acid → HCID 14835236、化合物

HRID 1084903ノート

反応式

HRID 1084903 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 14835236HCID 14835236、化合物

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-21b08dc909624e0fba376b4e870baa79
出典データセット
uspto-grants-1991_04
特許番号
US05006561

反応ノート

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