2-溴-5-氟甲苯 → 1-溴-4-氟-2-甲基-5-硝基苯

HRID 39195

反应方程式

HRID 39195 反应方程式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH3:9].F[B-](F)(F)F.[O:15]=[N+:16]=[O:17]>ClCCl>[Br:1][C:2]1[CH:7]=[C:6]([N+:16]([O-:17])=[O:15])[C:5]([F:8])=[CH:4][C:3]=1[CH3:9]

参与物

4

反应物 2

HCID 967432-溴-5-氟甲苯HCID 11073463四氟硼酸硝

产物 1

HCID 100369831-溴-4-氟-2-甲基-5-硝基苯收率 96.4%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

To a stirred solution of 1-bromo-4-fluoro-2-methyl-benzene (15.0 g, 79.8 mmol) in dichloromethane (300 mL) was added nitronium tetrafluoroborate (11.7 g, 87.8 mmol) in portions at 0° C. The mixture was heated at reflux for 5 h and was then poured into ice water. The organic layer was separated and the aqueous phase was extracted with dichloromethane (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and evaporated under reduced pressure to give crude 1-bromo-4-fluoro-2-methyl-5-nitrobenzene (18.0 g), which was used directly in the next step.

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 5 h
  3. customThe organic layer was separated
  4. extractionthe aqueous phase was extracted with dichloromethane (100 mL×3)
  5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  6. customevaporated under reduced pressure

来源与证据

ORD记录
ord-5f407a25c01940e38dcf5cc645b3817a
来源数据集
uspto-grants-2013_09
专利号
US08524767B2

关联笔记

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