反应 #1178395

ord-39aedc0acfff4a9188c51f4c2f5922cf

反应方程式

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
收率 83.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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