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1-Hexene → 5-Octyl-2-Norbornene 1-Hexene

HRID 2163750
ノート
印刷プレビュー

反応式

HRID 2163750 の反応式
[CH2:1]([CH:9]1[CH2:14][CH:13]2[CH2:15][CH:10]1[CH:11]=[CH:12]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH2:16]=[CH:17][CH2:18][CH2:19][CH2:20][CH3:21].[I-].C([Al+]CC)C>C1(C)C=CC=CC=1>[CH2:1]([CH:9]1[CH2:14][CH:13]2[CH2:15][CH:10]1[CH:11]=[CH:12]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH2:16]=[CH:17][CH2:18][CH2:19][CH2:20][CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 115971-HexeneHCID 15701270Bicyclo[2.2.1]hept-2-ene, 5-octyl-HCID 16686130AlEt2I

生成物 1

HCID 867362615-Octyl-2-Norbornene 1-Hexene

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

50 ml dry toluene cosolvent, 7 ml 5-octyl-2-norbornene (containing about 15 wt.% dicyclopentadiene trimer impurity), 8 ml 1-hexene solution and 0.6 ml diethylaluminum iodide solution were charged to a dry, nitrogen-purged 7 oz. bottle. 0.75 ml of the MoCl5 solution was charged last. After about 1 hour the reaction was shortstopped using a mixture of ethanolamine, Solution A and 2 ml of an antioxidant solution (0.1 g/ml of 2,2'-methylenebis-[4-methyl-6-t-butylphenol] in toluene). The polymer cement was coagulated using excess Solution A in a Waring blender. The solid recovered after being filtered and vacuum dried at 60° C. was found to be a terpolymer of octylnorbornene, dicyclopentadiene trimer and 1-hexene. Tg was measured and the value adjusted to compensate for the trimer impurity.

後処理

  1. custompurged 7 oz. bottle
  2. addition0.75 ml of the MoCl5 solution was charged last
  3. additiona mixture of ethanolamine, Solution A and 2 ml of an antioxidant solution (0.1 g/ml of 2,2'-methylenebis-[4-methyl-6-t-butylphenol] in toluene)
  4. customThe solid recovered
  5. filtrationafter being filtered
  6. customvacuum dried at 60° C.

出典と根拠

ORDレコード
ord-641a288bf93e4e5e94282f4aa29c39cc
出典データセット
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04136247

反応ノート

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