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1-Hexene → 5-Methyl-2-Norbornene 1-Hexene

HRID 2163746
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반응식

HRID 2163746 반응식
[CH3:1][CH:2]1[CH2:7][CH:6]2[CH2:8][CH:3]1[CH:4]=[CH:5]2.[CH2:9]=[CH:10][CH2:11][CH2:12][CH2:13][CH3:14].[I-].C([Al+]CC)C>C1C=CC=CC=1>[CH3:1][CH:2]1[CH2:7][CH:6]2[CH2:8][CH:3]1[CH:4]=[CH:5]2.[CH2:9]=[CH:10][CH2:11][CH2:12][CH2:13][CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 115971-HexeneHCID 101870Bicyclo[2.2.1]hept-2-ene, 5-methyl-HCID 16686130AlEt2I

생성물 1

HCID 867362545-Methyl-2-Norbornene 1-Hexene

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

500 ml dry benzene cosolvent, 74 ml 5-methyl-2-norbornene, 12 ml of the 1-hexene solution, and 6 ml of the diethylaluminum iodide solution were charged to a dry, nitrogen-purged quart bottle. 7.5 ml of the MoCl5 solution was charged last, and the bottle was shaken. After 80 minutes the reaction was shortstopped using a mixture of 1.5 ml ethanolamine, 10 ml of antioxidant solution (10 grams of 2,2',2"-tris[3(3,5-di-t-butyl-4-hydroxyphenyl)propionyloxy] ethyl isocyanurate in 100 ml benzene), and 1.5 ml Solution A. The polymer cement was coagulated using excess Solution A in a Waring blender. A solid weighing 66.0 grams was recovered after being filtered and vacuum dried at 60° C. It was found to be a ring-opened 5-methyl-2-norbornene/1-hexene copolymer having a DSV of about 1.90.

후처리

  1. custompurged quart bottle
  2. addition7.5 ml of the MoCl5 solution was charged last
  3. additiona mixture of 1.5 ml ethanolamine, 10 ml of antioxidant solution (10 grams of 2,2',2"-tris[3(3,5-di-t-butyl-4-hydroxyphenyl)propionyloxy] ethyl isocyanurate in 100 ml benzene), and 1.5 ml Solution A
  4. customwas recovered
  5. filtrationafter being filtered
  6. customvacuum dried at 60° C

출처 및 근거

ORD 기록
ord-95e9296371b9490b92adcb62952ff9be
출처 데이터셋
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04136247

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