Oxygen → Triphenylphosphine Oxide

HRID 328457

반응식

HRID 328457 반응식
[C:1]1([P:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O:22][Al](CC)CC)C.O=O>C/C(/[O-])=C/C(C)=O.C/C(/[O-])=C/C(C)=O.[Ni+2].C1C=CC([P]([Ni]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCOCC>[C:14]1([P:7](=[O:22])([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

참가 물질

7

반응물 3

HCID 977OxygenHCID 11776TriphenylphosphineHCID 16683109Ethoxydiethylaluminium

생성물 1

HCID 13097Triphenylphosphine Oxide

시약·촉매·용매 3

HCID 9834912Nickel(II) acetylacetonate촉매HCID 178420538HCID 178420538, 화합물촉매HCID 3283Diethyl Ether용매

실험 절차

10 gms. of nickel acetylacetonate and 40.95 gms. of triphenylphosphine are dissolved in 400 ml. of absolute ether and the solution is reduced with 16 ml. of ethoxydiethyl aluminum at 0° C. This results in a red-brown solution from which red-brown crystals precipitate after standing for 30 minutes. Complete precipitation of the crystals is achieved by cooling. The crystals are filtered with suction, washed with ether and dried. There are obtained 32 gms. (80% of the theoretical yield) of red-brown crystals, the elementary analysis of which agrees wit the formula Ni(P(C6H5)3)4. The compound is sensitive to air. When allowing oxygen to act on it, triphenylphosphine oxide is formed. The compound is capable of catalyzing the formation of cyclooctadiene from butadiene.

후처리

  1. customat 0° C
  2. customThis results in a red-brown solution from which red-brown crystals
  3. customprecipitate
  4. customComplete precipitation of the crystals
  5. temperatureby cooling
  6. filtrationThe crystals are filtered with suction
  7. washwashed with ether
  8. customdried
  9. customThere are obtained 32 gms
  10. custom(80% of the theoretical yield) of red-brown crystals

출처 및 근거

ORD 기록
ord-5a724e81ef2a4d38bd6c086366cd7920
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04017526

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