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2,3,5-Triiodobenzoic acid → 1-Decene

HRID 41779
ノート
印刷プレビュー

反応式

HRID 41779 の反応式
[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].C1C(I)=C(I)C(C(O)=O)=CC=1I.[H][H]>C1(C)C=CC=CC=1.CCCCCCC>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 69482,3,5-Triiodobenzoic acid2 回HCID 133811-DeceneHCID 178418361HCID 178418361、化合物

生成物 2

HCID 133811-DeceneHCID 15600Decane

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒4 回
HCID 8900
Heptane
溶媒

反応条件

温度
90 °C

実験手順

A solution of 100 g of purified 1-decene, 1.301 g of a TIBA stock solution (20 mg TIBA/g toluene solution) and 0.445 g of Metallocene A stock solution (1 mg Metallocene A/g toluene solution) was charged into a clean 600 ml autoclave equipped with an agitator, at room temperature. The reactor was then pressurized with 30 psig hydrogen. The mixture was then heated to 90° C. with stirring. A second solution made by adding a) 0.641 g of Activator A stock solution (1 mg Activator A/g toluene solution) and b) 20 g toluene solvent and was added and the reaction temperature was maintained at 90° C. overnight, then cooled down to room temperature, and any reactor pressure was vented. The liquid product was diluted with 50 ml heptane, stirred with 5 g activated alumina for half an hour and filtered to remove solids. The filtrate was analyzed by gas chromatography using an internal standard to obtain the wt % of normal-decane (n-C10) formation from 1-decene hydrogenation, wt % conversion to lubes and wt % lube yield. The lube product was then isolated by flashing the light ends (solvents, unreacted C10 fraction, and any fractions lighter than C30) and distilled at 180° C. under high vacuum (1 millitorr) for two hours to isolate the lube product.

後処理

  1. customequipped with an agitator, at room temperature
  2. additionwas added
  3. temperaturethe reaction temperature was maintained at 90° C. overnight
  4. temperaturecooled down to room temperature
  5. customany reactor pressure was vented
  6. stirringstirred with 5 g
  7. customfor half an hour
  8. filtrationfiltered
  9. customto remove solids

出典と根拠

ORDレコード
ord-70b03b60d66c4e9c88f474373cab2e3a
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08530712B2

反応ノート

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