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

HRID 2352053ノート

反応式

HRID 2352053 の反応式
[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]

参加物

4

反応物 2

HCID 4124402Phosphinic AcidHCID 124943393,4-Dimethoxyphenyltellurium trichloride

生成物 1

HCID 4345922Bis(3,4-dimethoxyphenyl)ditelluride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e043621f414a48caa772227eed0e3acd
出典データセット
uspto-grants-1989_10
特許番号
US04874866

反応ノート

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