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Triphenylphosphine → HCID 73794640, 화합물

HRID 1576130
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HRID 1576130 반응식
[I:1][CH2:2][CH2:3][CH:4]=[C:5]([CH3:8])[CH:6]=[CH2:7].[C:9]1([P:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[I-].[PH4+]>C1C=CC=CC=1>[I-:1].[CH3:8][C:5]([CH:6]=[CH2:7])=[CH:4][CH2:3][CH2:2][P+:15]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11776TriphenylphosphineHCID 166618Phosphonium iodideHCID 53950976HCID 53950976, 화합물

생성물 1

HCID 73794640HCID 73794640, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of 89.0 g. (0.40 mole) of iodo-4-methyl-3,5-hexadiene, 105 g. (0.40 mole) of triphenylphosphine and 350 ml. of benzene was stirred and refluxed for 8 hours. The solvent was removed in vacuo. After addition of about 1 1. of ether the oily mixture was left for one day at 0°. The crystallized salt was suction filtered, finely grinded and washed with ether, then dried for 4 hours at 80°/0.01 Torr. Obtained: 140 g. of phosphonium iodide, m.p. 124°-128°.

후처리

  1. additionA mixture of 89.0 g
  2. temperaturerefluxed for 8 hours
  3. customThe solvent was removed in vacuo
  4. additionAfter addition of about 1 1
  5. filtrationfiltered
  6. customfinely grinded
  7. washwashed with ether
  8. customdried for 4 hours at 80°/0.01 Torr
  9. customObtained

출처 및 근거

ORD 기록
ord-81e852bf653d4ee3bc0feccce5dcbb3b
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03979425

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