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Isoprene → 2-Methylbuta-1,3-diene;styrene

HRID 718481
ノート
印刷プレビュー

反応式

HRID 718481 の反応式
CN(CCN(C)C)C.[CH2:9]=[CH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C([Li])CCC.C=CC(=C)C>C1CCCCC1>[CH2:9]=[CH:10][C:11](=[CH2:12])[CH3:16].[CH2:9]=[CH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
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

6

反応物 4

HCID 6557Isoprene2 回HCID 7501Styrene2 回HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 178418339Butyllithium

生成物 1

HCID 1599892-Methylbuta-1,3-diene;styrene

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

反応条件

温度
40 °C

実験手順

In a pressure-resistant reactor, 23.3 kg of cyclohexane, 2.6 millimoles of TMEDA, and 1.35 kg of styrene were introduced, and while the content was stirred at 40° C., 86 millimoles of n-butyllithium was added thereto. Polymerization was carried out for one hour while the temperature was increased to 50° C. The polymerization conversion ratio of styrene was 100%. Subsequently, 7.1 kg of isoprene was continuously added to the reactor over one hour while the temperature was controlled to be maintained at 50° C. to 60° C. After the addition of isoprene was completed, polymerization was carried out for another one hour, and thus a styrene-isoprene block copolymer was formed. The polymerization conversion ratio of isoprene was 100%. Thereafter, 172 millimoles of methanol as a polymerization terminator was added thereto and mixed thoroughly therein, and thus the reaction was terminated. Incidentally, the amounts of the various reagents used in the reaction are summarized in Table 1. The reaction liquid obtained as described above was treated in the same manner as in Production Example 1, and thus a composition of Production Example 6 (block copolymer) was collected. Furthermore, a portion of the reaction liquid thus obtained was taken, and the same measurements as in Production Example 1 were carried out. These measurement values are presented in Table 2.

後処理

  1. customPolymerization
  2. temperaturewas increased to 50° C
  3. temperatureto be maintained at 50° C. to 60° C
  4. custompolymerization
  5. waitwas carried out for another one hour

出典と根拠

ORDレコード
ord-53ad9b1b51f0478a8bcee6985599dfc7
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09193893B2

反応ノート

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