反応 #1178395

ord-39aedc0acfff4a9188c51f4c2f5922cf

反応方程式

O=C(c1ccc(O)cc1)c1ccc(O)cc1
4,4′-dihydroxybenzophenone
Oc1ccc(C(=C(c2ccc(O)cc2)c2ccc(O)cc2)c2ccc(O)cc2)cc1
1,1,2,2-tetrakis(4-hydroxyphenyl)ethylene
収率 83.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was refluxed for 20 h
  2. 2
    ろ過filtered
  3. 3
    その他The filtrates were evaporated
  4. 4
    その他the crude product was purified by a silica gel column
  5. 5
    その他DHTPE was obtained as slight yellow powder of 83% yield

実験手順

A suspension of 4,4′-dihydroxybenzophenone (3.0 g, 14.0 mmol), 1 equiv of TiCl4 (1.54 ml, 14.0 mmol), and 2 equiv of Zn dust (1.83 g, 28.0 mmol) in 100 ml of dry THF was refluxed for 20 h. The reaction mixture was cooled to room temperature and filtered. The filtrates were evaporated and the crude product was purified by a silica gel column using ethyl acetate (EA) as eluent. DHTPE was obtained as slight yellow powder of 83% yield.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08129111B2uspto-grants-2012_03