海萝胶 → HCID 12902867，化合物

HRID 128090

反应方程式

HRID 128090 反应方程式
[C:1]1([C:7]2[C:11]3[CH:12]=[C:13]([C:16]4[CH:24]=[CH:23][C:19]([C:20]([OH:22])=[O:21])=[CH:18][CH:17]=4)[CH:14]=[CH:15][C:10]=3[O:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N+:25]([O-:30])([N+]([O-])=O)=[O:26].C(Cl)(Cl)Cl.Cl>[OH-].[Na+]>[N+:25]([C:8]1[O:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:17]=[CH:18][C:19]([C:20]([OH:22])=[O:21])=[CH:23][CH:24]=3)=[CH:12][C:11]=2[C:7]=1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)([O-:30])=[O:26]

参与物

6

反应物 4

HCID 313海萝胶HCID 6212三氯甲烷HCID 25352四氧化二氮HCID 23455894HCID 23455894，化合物

产物 1

HCID 12902867HCID 12902867，化合物

试剂、催化剂与溶剂 1

HCID 14798二甲基对苯二胺二盐酸溶剂

实验过程

A solution of 3.1 g. (0.01 mole) of the product of step D and 2 g. of dinitrogen tetraoxide in 250 ml. of chloroform is stirred at about 20° C. for about 16 hours. Evaporation of the mixture provides a residue which is dissolved in 10 percent sodium hydroxide solution, then acidified with hydrochloric acid. The precipitate is collected by filtration, dissolved in a chloroform/ethanol mixture and chromatographed on silica gel, eluting with chloroform. The solid obtained is recrystallized twice from a mixture of water and N,N-dimethylformamide to provide yellow crystals of 4-(2-nitro-3-phenylbenzofuran-5-yl)benzoic acid, m.p. 259°-261° C.

后处理

  1. customEvaporation of the mixture
  2. customprovides a residue which
  3. filtrationThe precipitate is collected by filtration
  4. dissolutiondissolved in a chloroform/ethanol mixture
  5. customchromatographed on silica gel
  6. washeluting with chloroform
  7. customThe solid obtained
  8. customis recrystallized twice from a mixture of water and N,N-dimethylformamide

来源与证据

ORD记录
ord-2f2e1cf6295e4bb59c5f958e86004c06
来源数据集
uspto-grants-1981_03
专利号
US04258213

关联笔记

加载中…