六水硝酸铽 → 6-硝基-4-二氢色原酮

HRID 862425笔记

反应方程式

HRID 862425 反应方程式
[O:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[CH2:3][CH2:2]1.[N+:12]([O-])([OH:14])=[O:13]>>[N+:12]([C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[O:1][CH2:2][CH2:3][C:4]2=[O:11])([O-:14])=[O:13]

参与物

3

反应物 2

HCID 944六水硝酸铽HCID 681102,3-二氢苯并吡喃-4-酮

产物 1

HCID 52288316-硝基-4-二氢色原酮

实验过程

Fuming nitric acid (200 ml) was cooled to from -30° to -35° C. and 4-chromanone (29.0 g) was added with stirring over 30 minutes. The mixture was further stirred for 30 minutes at the intact temperature and successively poured into ice water. The resulting mixture was extracted with ethyl acetate (2,500 ml). The organic layer was dried with anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to obtain the crude product as a yellow solid. The crude product was washed with a solvent mixture, n-hexane:ethyl acetate=1:1, to obtain 6-nitro-4-chromanone (27.0 g).

后处理

  1. additionwas added
  2. stirringThe mixture was further stirred for 30 minutes at the intact temperature
  3. extractionThe resulting mixture was extracted with ethyl acetate (2,500 ml)
  4. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customto obtain the crude product as a yellow solid
  7. washThe crude product was washed with a solvent mixture, n-hexane

来源与证据

ORD记录
ord-2232ac656e184c4ea27da9d00d462c44
来源数据集
uspto-grants-1998_02
专利号
US05719145

反应笔记

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