Phosphinic Acid → Bis(3,4-dimethoxyphenyl)ditelluride

HRID 543065노트

반응식

HRID 543065 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([Te:11](Cl)(Cl)Cl)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[PH2](O)=O>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([Te:11][Te:11][C:5]2[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

4

반응물 2

HCID 4124402Phosphinic AcidHCID 124943393,4-Dimethoxyphenyltellurium trichloride

생성물 1

HCID 4345922Bis(3,4-dimethoxyphenyl)ditelluride

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3,4-Dimethoxyphenyltellurium trichloride (37.2 g=0.1 mole) was dissolved in absolute ethanol (500 ml), and the slightly turbid solution was filtered. To the rapidly stirred solution was added, at room temperature, 50% aqueous hypophosphorous acid (30 ml, ≃0.3 mole) as rapidly as possible. There was a brief appearance of a brown solution color, before the entire solution set to a mass of black fibrous crystals. The product was collected after 15 minutes by filtration using rubber dam to compact the highly solvated crystal mass. The product was washed with water and then air dried to yield 25.2 g, 95% of theory, black fibrous crystals, m.p. 134°-136° C. Recrystallization from isopropanol raised the m.p. to 136°-139° C. C, H and Te elemental analyses were in agreement with the structural formula.

후처리

  1. filtrationthe slightly turbid solution was filtered
  2. additionTo the rapidly stirred solution was added, at room temperature
  3. filtrationThe product was collected after 15 minutes by filtration
  4. washThe product was washed with water
  5. customair dried
  6. customto yield 25.2 g, 95% of theory, black fibrous crystals, m.p. 134°-136° C
  7. customRecrystallization from isopropanol
  8. temperatureraised the m.p. to 136°-139° C

출처 및 근거

ORD 기록
ord-437a0c1648904372956c2201c28c761b
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04661438

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