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

HRID 613958

반응식

HRID 613958 반응식
[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

참가 물질

7

반응물 4

HCID 241BenzeneHCID 8471TriethylamineHCID 24811TrichlorosilaneHCID 867345011,2-Bis(o-anisylphenylphosphinyl) ethane2회

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 6342Acetonitrile용매

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.

후처리

  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

출처 및 근거

ORD 기록
ord-57e71f35f7214d6da13abd879da00e45
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04142992

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