六水硝酸铽 → 5-Bromo-4-fluoro-2-nitrobenzonitrile

HRID 17530笔记

反应方程式

HRID 17530 反应方程式
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[C:5]#[N:6].[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[Br:1][C:2]1[C:9]([F:10])=[CH:8][C:7]([N+:11]([O-:13])=[O:12])=[C:4]([CH:3]=1)[C:5]#[N:6]

参与物

4

反应物 2

HCID 944六水硝酸铽HCID 1235793-溴-4-氟苯甲腈

产物 1

HCID 685846195-Bromo-4-fluoro-2-nitrobenzonitrile收率 48%

试剂、催化剂与溶剂 1

HCID 1118四氧化硫溶剂

实验过程

3-Bromo-4-fluorobenzonitrile (25 g, 0.125 mol) was dissolved in concentrated sulfuric acid (200 ml), and at 0° C., fuming nitric acid was dropwise added at 0° C., taking 1 hour. After stirred for 30 minutes at the same temperature, this was heated up to room temperature, taking 1.5 hours. This was gradually poured into ice. The formed precipitate was collected by filtration with washing with water, and dried under reduced pressure. The collected yellow powder was fractionated with chloroform and aqueous 1 M sodium hydroxide solution. The organic layer was washed with saturated brine, then dried over anhydrous sodium sulfate. The solvent was evaporated away, and the resulting residue was well dried under reduced pressure to obtain the entitled compound (14.7 g, 48%) as a yellow powder.

后处理

  1. customat 0° C.
  2. additionwas dropwise added at 0° C.
  3. waittaking 1.5 hours
  4. additionThis was gradually poured into ice
  5. filtrationThe formed precipitate was collected by filtration
  6. washwith washing with water
  7. customdried under reduced pressure
  8. washThe organic layer was washed with saturated brine
  9. dry with materialdried over anhydrous sodium sulfate
  10. customThe solvent was evaporated away
  11. customthe resulting residue was well dried under reduced pressure

来源与证据

ORD记录
ord-3e240567bde4449c8214003cc724eb2f
来源数据集
uspto-grants-2010_06
专利号
US07737166B2

反应笔记

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