O-Xylene → 4,4'-DIVINYLBIPHENYL

HRID 1857085노트

반응식

HRID 1857085 반응식
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]

참가 물질

5

반응물 3

HCID 7237O-XyleneHCID 73814-tert-ButylcatecholHCID 618022HCID 618022, 화합물2회

생성물 1

HCID 109874454,4'-DIVINYLBIPHENYL

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-b9fda63a35624064a4208182473a397e
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06143922

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