1-Eicosene → Undecylenyl Iodide Eicosene

HRID 373755

반응식

HRID 373755 반응식
[CH2:1]([I:12])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH:10]=[CH2:11].[CH2:13]=[CH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32].[Cl-].C([Al+]CC)C.CO.Cl>C1(C)C=CC=CC=1.CO>[CH2:1]([I:12])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH:10]=[CH2:11].[CH2:13]=[CH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32]

참가 물질

7

반응물 4

HCID 189361-EicoseneHCID 1111946211-Iodoundec-1-eneHCID 16686102Diethyl aluminum chlorideHCID 21893726Hydrochloride methanol

생성물 1

HCID 131717650Undecylenyl Iodide Eicosene수율 166.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 1140Toluene용매2회

실험 절차

To a glass screw top jar were added undecylenyl iodide (6.3 grams), toluene solvent (63.1 grams), and eicosene (18.73 grams). Under argon atmosphere were added diethyl aluminum chloride (25 milliliters of a 1.8 molar solution in toluene) and 1.25 teaspoons of TiCl3 --AA (available from Alfa, about 5 grams). The sealed jar was stirred for 2 hours. Methanol was added dropwise until the mixture turned green. The reaction mixture was then added to methanol/hydrochloric acid in a Waring blender to precipitate the solid polymer. In the blender, the polymer was washed successively with methanol, water and then methanol. After filtration, the isolated polymer was dried in vacuo to yield 21.04 grams of the semicrystalline polymer product, poly(undecylenyl iodide-eicosene) copolymer, the DSC of this product indicated two semicrystalline endotherms at 30° and 55° C. Solid state 13C NMR analysis measured 17 weight percent of CH2 --I groups present.

후처리

  1. customto precipitate the solid polymer
  2. washIn the blender, the polymer was washed successively with methanol, water
  3. filtrationAfter filtration
  4. customthe isolated polymer was dried in vacuo

출처 및 근거

ORD 기록
ord-131e292e81bd46ebbb84c6b2b725a088
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166026

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