O-Xylene → 4,4'-DIVINYLBIPHENYL

HRID 1857085ノート

反応式

HRID 1857085 の反応式
O[CH:2]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([CH:16](O)[CH3:17])=[CH:12][CH:11]=2)=[CH:6][CH:5]=1)[CH3:3].C(C1C=C(O)C(=CC=1)O)(C)(C)C.CC1C=CC=CC=1C>O>[CH:2]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([CH:16]=[CH2:17])=[CH:12][CH:11]=2)=[CH:6][CH:5]=1)=[CH2:3]

参加物

5

反応物 3

HCID 7237O-XyleneHCID 73814-tert-ButylcatecholHCID 618022HCID 618022、化合物2 回

生成物 1

HCID 109874454,4'-DIVINYLBIPHENYL

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The mixture of 5.0020 g (0.02064 mole) of 4,4'-di-(1-hydroxyethyl)biphenyl (DHEBP), 0.0050 g (0.1% of DHEBP weight) of 4-tert-butyl catechol, 00742 g (1.483% of DHEBP weight or 4.11 mmol/L) of TSA, and 90 mL of o-xylene was heated at the boiling temperature for 40 minutes. Water released during the dehydration was azeotroped from the system. Then, the reaction mixture was treated as described in Example 1. The yield of the unsaturated composition riched with 4,4 '-divinylbiphenyl (DVBP) was 3.8 g (89.3% of theor.). According to reversed phase chromatography, the content of components was as follows, wt-%: Monomer M1 (DVBP) 77, its unsaturated dimer 17, its insaturated trimer 5%, tetramers and higher oligomers <1%. The pure DVBP (purity was >99.5%), mp 150-153° C. was obtained by sublimation of the monomer at 160° C. for 1 hour under vacuum (1-2 mm Hg).

後処理

  1. temperaturewas heated at the boiling temperature for 40 minutes
  2. customwas azeotroped from the system
  3. additionThen, the reaction mixture was treated

出典と根拠

ORDレコード
ord-b9fda63a35624064a4208182473a397e
出典データセット
uspto-grants-2000_11
特許番号
US06143922

反応ノート

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