苯 → 2-氯-4-氟硝基苯

HRID 65328

反应方程式

HRID 65328 反应方程式
[Cl:1][C:2]1[CH:3]=[C:4]([F:8])[CH:5]=[CH:6][CH:7]=1.S(=O)(=O)(O)O.[N+:14]([O-])([OH:16])=[O:15].C1C=CC=CC=1>CCCCCC>[Cl:1][C:2]1[CH:3]=[C:4]([F:8])[CH:5]=[CH:6][C:7]=1[N+:14]([O-:16])=[O:15]

参与物

6

反应物 4

HCID 241苯HCID 944六水硝酸铽HCID 1118四氧化硫HCID 2230873-氯氟苯

产物 1

HCID 750172-氯-4-氟硝基苯收率 16.7%

试剂、催化剂与溶剂 1

HCID 8058正己烷溶剂

实验过程

m-Chlorofluorobenzene (240 g. 1.85 moles) is added to a mixture of sulfuric acid (185 g. 1.85 moles) and nitric acid (166 g., 1.85 moles) at -5° C. in 3.5 hours, stirred 13 hours, then benzene (200 ml.) and hexane (200 ml.) are added. The extract is washed with water (1×300 ml.), sodium carbonate solution (1×300 ml.), and water (1×300 ml.), dried and the solvents removed. The residue is distilled to give 138 g. of mixture isomers. The 4-nitro isomer crystallizes and is filtered off to give 3-chloro-4-nitrofluorobenzene (51 g. 16.7%) m.p. 36°-38° C.

后处理

  1. washThe extract is washed with water (1×300 ml.), sodium carbonate solution (1×300 ml.), and water (1×300 ml.)
  2. customdried
  3. customthe solvents removed
  4. distillationThe residue is distilled
  5. customto give 138 g
  6. customThe 4-nitro isomer crystallizes
  7. filtrationis filtered off

来源与证据

ORD记录
ord-355d292c1c8444b6a63c811435ffb1f9
来源数据集
uspto-grants-1986_09
专利号
US04613360

关联笔记

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