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

HRID 1164699ノート

反応式

HRID 1164699 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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°).

後処理

  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)

出典と根拠

ORDレコード
ord-f5fd751ccfe84171b1e16e14271679c0
出典データセット
uspto-grants-1983_01
特許番号
US04370497

反応ノート

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