六水硝酸铽 → HCID 14835236，化合物

HRID 1761869笔记

反应方程式

HRID 1761869 反应方程式
[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]

参与物

3

反应物 2

HCID 944六水硝酸铽HCID 14835235N-(2,3-Dihydro-1H-inden-2-yl)formamide

产物 1

HCID 14835236HCID 14835236，化合物

实验过程

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°.

后处理

  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

来源与证据

ORD记录
ord-d8c42301746f4f1592e224c2da08dc75
来源数据集
uspto-grants-1989_05
专利号
US04829071

反应笔记

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