Hydrochloric Acid → HCID 12902867, 화합물

HRID 128090

반응식

HRID 128090 반응식
[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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 25352Nitrogen oxide (N2O4)HCID 23455894HCID 23455894, 화합물

생성물 1

HCID 12902867HCID 12902867, 화합물

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2f2e1cf6295e4bb59c5f958e86004c06
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04258213

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