O-Xylene → 4,4'-DIVINYLBIPHENYL

HRID 1384443노트

반응식

HRID 1384443 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-b07999b14bd944dd9f66f75ef7757183
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06258909B1

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