2,4-二氯酚 → 2-Chloro-4-(2',4'-dichlorophenoxy)benzonitrile

HRID 436982

反应方程式

HRID 436982 反应方程式
[Cl:1][C:2]1[CH:9]=[C:8](Cl)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[K].[Cl:12][C:13]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:14]=1[OH:20]>CC(N(C)C)=O>[Cl:1][C:2]1[CH:9]=[C:8]([O:20][C:14]2[CH:15]=[CH:16][C:17]([Cl:19])=[CH:18][C:13]=2[Cl:12])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5]

参与物

5

反应物 3

HCID 84492,4-二氯酚HCID 810502,4-二氯苯腈HCID 5462222钾

产物 1

HCID 214295702-Chloro-4-(2',4'-dichlorophenoxy)benzonitrile

试剂、催化剂与溶剂 1

HCID 31374N,N-二甲基乙酰胺溶剂

实验过程

A stirred solution of 2,4-dichlorobenzonitrile (51.6 g., 0.03 mole) and the potassium salt of 2,4-dichlorophenol (60.3 g., 0.03 mole) in 250 ml. of dimethyl acetamide was heated for 24 hours at 120° C. The cooled reaction mixture was diluted with 1000 ml. of water and the resultant oil was extracted with ether. Evaporation of the ether solution gave 88.0 g. of brown oil. Analysis by v.p.c. showed a 2:1 mixture of the desired compound and the isomeric 4-chloro-2-(2',4'-dichlorophenoxy) benzonitrile. A series of fractional crystallizations from 60°-110° C. petroleum ether gave the desired 2-chloro-4-(2',4'-dichlorophenoxy)benzonitrile with a melting point of 69°-74° C. The minor isomeric by-product melted at 110°-113° C.

后处理

  1. customThe cooled reaction mixture
  2. additionwas diluted with 1000 ml
  3. extractionof water and the resultant oil was extracted with ether
  4. customEvaporation of the ether solution
  5. customgave 88.0 g

来源与证据

ORD记录
ord-b9edb5826b9c484285f87d566eff734b
来源数据集
uspto-grants-1977_06
专利号
US04029493

关联笔记

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