Benzene → 1,2-Bis(o-anisylphenylphosphino) ethane

HRID 436350

反応式

HRID 436350 の反応式
[CH2:1]([P:10]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([CH2:12][CH2:13][P:14]([CH2:22][C:23]1[C:24]([O:29][CH3:30])=[CH:25][CH:26]=[CH:27][CH:28]=1)([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=O)=O)[C:2]1[C:3]([O:8][CH3:9])=[CH:4][CH:5]=[CH:6][CH:7]=1.Cl[SiH](Cl)Cl.C(N(CC)CC)C.C1C=CC=CC=1>CO.C(#N)C>[CH2:1]([P:10]([C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)[CH2:12][CH2:13][P:14]([CH2:22][C:23]1[C:24]([O:29][CH3:30])=[CH:25][CH:26]=[CH:27][CH:28]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:2]1[C:3]([O:8][CH3:9])=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 4

HCID 241BenzeneHCID 8471TriethylamineHCID 24811TrichlorosilaneHCID 867345011,2-Bis(o-anisylphenylphosphinyl) ethane2 回

生成物 1

HCID 150615581,2-Bis(o-anisylphenylphosphino) ethane

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6342Acetonitrile溶媒

実験手順

Reduction of 1,2-bis(o-anisylphenylphosphinyl) ethane was accomplished by refluxing 16.5 g. (.12 mole) trichlorosilane and 12.2 g. (.12 mole) triethylamine in 188 ml. of dry benzene for one hour. Then 3.0 g. (.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.

後処理

  1. temperatureby refluxing 16.5 g
  2. temperaturethe mixture refluxed 1.5 hours
  3. customQuenching in 30% sodium hydroxide solution
  4. customby separating
  5. customevaporating the organic layer
  6. customgave 1.4 g
  7. customFurther crystallization from hot methanol

出典と根拠

ORDレコード
ord-907d81b6612b48c0bc4d1749cb8cd83e
出典データセット
uspto-grants-1977_02
特許番号
US04008281

関連ノート

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