Potassium Carbonate → Benzene, 1,1'-tellurobis[4-methoxy-

HRID 1164699노트

반응식

HRID 1164699 반응식
N(C1C=CC(C(O)=O)=CC=1)N.[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([Te:20]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=2)=O)=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)Cl>[CH3:29][O:28][C:25]1[CH:24]=[CH:23][C:22]([Te:20][C:17]2[CH:18]=[CH:19][C:14]([O:13][CH3:12])=[CH:15][CH:16]=2)=[CH:27][CH:26]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 120894-Hydrazinobenzoic acidHCID 3044917Bis(p-methoxyphenyl) telluroxide

생성물 1

HCID 4605422Benzene, 1,1'-tellurobis[4-methoxy-수율 44%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

p-Hydrazino benzoic acid (152 mg, 1 mmol) and bis-(p-methoxyphenyl)-telluroxide (394 mg, 1.10 mmol) were stirred in chloroform (10 ml) at room temperature for 24 h. The reaction mixture was then poured into saturated aqueous potassium carbonate, the phases separated and the aqueous phase extracted with dichloromethane (2×10 ml). The combined organic phases were dried over sodium sulphate and evaporated under reduced pressure. The residue after purification by column chromatography (chloroform) gave bis-(p-methoxyphenyl)-telluride (151 mg, 44%). The aqueous phase, on acidification with hydrochloric acid and extraction with dichloromethane gave a yellow solid (54 mg) which on sublimation under reduced pressure gave pure benzoic acid (32 mg, 26%) m.p. 122° (lit., 122°).

후처리

  1. customthe phases separated
  2. extractionthe aqueous phase extracted with dichloromethane (2×10 ml)
  3. dry with materialThe combined organic phases were dried over sodium sulphate
  4. customevaporated under reduced pressure
  5. customThe residue after purification by column chromatography (chloroform)

출처 및 근거

ORD 기록
ord-f5fd751ccfe84171b1e16e14271679c0
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04370497

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