反应 #1596952

ord-1475262ba7e045a3a7e2a397513bdafa

反应方程式

BrCCBr
1,2-dibromoethane
CCCCCC.[Li][CH2]CCC
n-butyl lithium hexane
C1CCOC1
THF
c1ccc2c(c1)oc1ccccc12
dibenzofuran
Brc1cccc2oc3ccccc3c12
Compound 16-1
Brc1cccc2oc3ccccc3c12
Bromodibenzofuran

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The obtained solution is again cooled to −78° C.
  2. 2
    温度the temperature of the solution is raised to room temperature over 120 minutes
  3. 3
    其他the reaction
  4. 4
    萃取Organic layers extracted from the obtained mixture with ethyl acetate
  5. 5
    干燥are dried with sodium sulfate
  6. 6
    浓缩concentrated with an evaporator

实验过程

Under nitrogen current at −78° C., an n-butyl lithium hexane solution (1.6M, 69 ml) is dropped to a THF solution (175 ml) containing 16.82 g of dibenzofuran, and the temperature of the mixture is raised to room temperature over 80 minutes. The obtained solution is again cooled to −78° C., 19.0 ml of 1,2-dibromoethane is added to the solution, and the temperature of the solution is raised to room temperature over 120 minutes. Water is added to the obtained reaction solution to stop the reaction. Organic layers extracted from the obtained mixture with ethyl acetate are dried with sodium sulfate, and then concentrated with an evaporator to obtain 12.35 g of Compound 16-1.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08211551B2uspto-grants-2012_07