반응 #55324

반응 방정식

1,2-bis(o-anisylphenylphosphinyl) ethane

1,2-bis(o-anisylphenylphosphinyl) ethane

triethylamine

benzene

trichlorosilane

→

1,2-bis(o-anisylphenylphosphino) ethane

용매

methanol

acetonitrile

반응 조건

후처리

1. 1
   온도by refluxing 16.5 g
2. 2
   온도the mixture refluxed 1.5 hours
3. 3
   기타Quenching in 30% sodium hydroxide solution
4. 4
   기타by separating
5. 5
   기타evaporating the organic layer
6. 6
   기타gave 1.4 g
7. 7
   기타Further crystallization from hot methanol

실험 절차

Reduction of 1,2-bis(o-anisylphenylphosphinyl) ethane was accomplished by refluxing 16.5 g. (0.12 mole) trichlorosilane and 12.2 g. (0.12 mole) triethylamine in 188 ml. of dry benzene for one hour. Then 3.0 g. (0.012 mole) of 1,2-bis(o-anisylphenylphosphinyl) ethane in 75 ml. of dry acetonitrile was added and the mixture refluxed 1.5 hours. Quenching in 30% sodium hydroxide solution followed by separating and evaporating the organic layer gave 1.4 g. of crude crystals which were insoluble in cold methanol. Further crystallization from hot methanol gave 1,2-bis(o-anisylphenylphosphino) ethane, m.p. 102°-104° C., [α]D20 -83.4° (C=0.5 in CHCl3). The mass spectra gave a very strong parent peak at 458 and the nmr confirmed the structure.

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