Nitrogen → Benzene, ethenyl-, polymer with 1,3-butadiene

HRID 16723

反応式

HRID 16723 の反応式
[CH2:1]=[CH:2][CH:3]=[CH2:4].[CH2:5]=[CH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[Li]CCCC.C1(C(C2C=CC=CC=2)=C)C=CC=CC=1.N#N.Cl[Sn](Cl)(Cl)Cl>CCCCCC>[CH2:1]=[CH:2][CH:3]=[CH2:4].[CH2:5]=[CH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

8

反応物 6

HCID 947NitrogenHCID 7501StyreneHCID 78451,3-ButadieneHCID 107401,1-Diphenylethylene2 回HCID 24287Tin tetrachloride2 回HCID 178418339Butyllithium

生成物 1

HCID 62697Benzene, ethenyl-, polymer with 1,3-butadiene

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒3 回

実験手順

To a 1-gallon stainless steel reactor under a N2 blanket was charged 3.0 lbs. of 21.5% 1,3-butadiene in technical grade hexane, 3.0 lbs. of technical grade hexane and 67 g of 33% styrene in hexane. All solvents were dried to less than 5 ppm water and oxygen free. 64.7 mmol of nBuLi was charged to the reactor and polymerization was allowed to proceed for 5 and ⅓ hours at 123-127° F. 308 grams of a control sample was taken and live cement was terminated with isopropanol. A second 308 gram sample was also taken. It was calculated that a maximum of 51.3 mmol of carbon-bound lithium was still present in the reactor, 50.4 mmol of 1,1-diphenylethylene and 16 mmol of the vinyl modifier 2,2-di(tetrahydrofuryl)propane were added to the reactor and allowed to react for 2.75 hours at 125° F. and a further 16 hours at ˜70° F. A sample was taken for analysis and it was determined that 23.6% of the 1,1-diphenylethylene remained unreacted. A 306 gram sample was taken in a N2 purged crown-capped bottle and 1.7 mmol SnCl4 were added to terminated and couple the polymer. (It was calculated that a maximum of 0.021 mmol carbon-bound lithium was present per gram of cement.) Both the control sample and the SnCl4 coupled sample were worked up by evaporating the hexane in a rotoevaporator and finishing in a vacuum oven at 50° C. Molecular weight analysis results by Gel Permeation Chromatography (GPC) are shown in Table 3.

後処理

  1. additionTo a 1-gallon stainless steel reactor under a N2 blanket was charged 3.0 lbs
  2. dry with materialAll solvents were dried to less than 5 ppm water and oxygen free
  3. customto proceed for 5 and ⅓ hours at 123-127° F
  4. customlive cement was terminated with isopropanol
  5. additionwere added to the reactor
  6. customto react for 2.75 hours at 125° F. and a further 16 hours at ˜70° F
  7. custompurged
  8. additionwere added
  9. customto terminated
  10. customby evaporating the hexane in a rotoevaporator
  11. customfinishing in a vacuum oven at 50° C
  12. customMolecular weight analysis results by Gel Permeation Chromatography (GPC)

出典と根拠

ORDレコード
ord-4b15a74b8f3b4719813c53862261102f
出典データセット
uspto-grants-2010_06
特許番号
US07737218B2

関連ノート

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