Benzene → Styrene t-butylstyrene

HRID 1578834ノート

反応式

HRID 1578834 の反応式
C1C=CC=CC=1.C([Li])CCC.[C:12]([CH:16]=[CH:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([CH3:15])([CH3:14])[CH3:13].[CH2:24]=[CH:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>CCCCCCC.CO>[C:12]([CH:16]=[CH:17][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)([CH3:15])([CH3:13])[CH3:14].[CH2:24]=[CH:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

参加物

7

反応物 4

HCID 241BenzeneHCID 7501Styrene3 回HCID 138033tert-Butylstyrene4 回HCID 178418339Butyllithium

生成物 1

HCID 86733069Styrene t-butylstyrene

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 8900Heptane溶媒

実験手順

Under anaerobic and anhydrous conditions 400 ml of purified benzene is charged to a polymerization vessel followed by 0.53 milliequivalents of n-butyllithium in heptane. t-Butylstyrene (9.0 g, 0.056 mole) is added at about 30°C., and the resultant solution is stirred 15-30 minutes at 30°-60°C. Six more monomer additions are made as follows: styrene (18.0 g, 0.173 mole), t-butylstyrene (9.0 g), styrene (18.0 g), t-butylstyrene (9.0 g), styrene (18.0 g), and t-butylstyrene (9.0 g). Between additions the solution is permitted to stir for 15-30 minutes at 30°-60°C. The polymerization solution is then inactivated by the addition of a small quantity of methanol, and the seven block copolymer is isolated by precipitation with methanol in a Waring blender. The precipitated block copolymer is thoroughly washed with methanol and vacuum oven dried at 80°C. for 24 hours. A quantitative yield (90 g) of block copolymer is obtained. Gel permeation chromatography shows the copolymer to possess a narrow molecular weight distribution. A molded film of the block copolymer is clear and transparent. The calculated degree of polymerization of the seven block copolymer is 1400, and the calculated molecular weight is 170,000.

後処理

  1. washThe precipitated block copolymer is thoroughly washed with methanol and vacuum oven
  2. customdried at 80°C. for 24 hours
  3. customA quantitative yield (90 g) of block copolymer is obtained
  4. customThe calculated degree of polymerization of the seven block copolymer

出典と根拠

ORDレコード
ord-2608e57d703543539a5f35663c3978ab
出典データセット
uspto-grants-1976_02
特許番号
US03939242

反応ノート

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