反应 #2314312

ord-fa3931b1f7fd4f1ea086ee8953de38b7

反应方程式

O=C([O-])[O-].[K+].[K+]
K2CO3
O=c1nc2c(-c3ccccc3)c(-c3ccccc3)nc-2c1=O
diphenyl-diketopyrrolopyrrole
O=c1nc2c(-c3ccccc3)c(-c3ccccc3)nc-2c1=O
DPP
BrCc1ccccc1
benzyl bromide
O=C1C(=O)N(Cc2ccccc2)c2c(-c3ccccc3)c(-c3ccccc3)n(Cc3ccccc3)c21
orange solid
收率 101.3%
O=C1C(=O)N(Cc2ccccc2)c2c(-c3ccccc3)c(-c3ccccc3)n(Cc3ccccc3)c21
N,N′-dibenzyl-diphenyl-diketopyrrolopyrrol
收率 101.3%

溶剂

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A 100 ml round-bottom flask equipped with a stirrer
  2. 2
    温度reflux condenser
  3. 3
    温度The slurry is cooled
  4. 4
    其他the orange solid is isolated by filtration
  5. 5
    洗涤The solid is washed with water and MeOH
  6. 6
    workup.DISSOLUTIONby dissolving in hot CHCl3
  7. 7
    其他After condensation

实验过程

A 100 ml round-bottom flask equipped with a stirrer and reflux condenser is charged with 1.47 g (5.1 mmol) of diphenyl-diketopyrrolopyrrole (hereinafter referred to DPP), 3.44 g (20.1 mmol) of benzyl bromide, 1.38 g (10.0 mmol) of K2CO3 and 50 ml of DMF. Under nitrogen atmosphere, the mixture is stirred and heated at 100° C. for 42.5 hours. The slurry is cooled and the orange solid is isolated by filtration. The solid is washed with water and MeOH, followed by dissolving in hot CHCl3. This CHCl3 solution is applied to silica gel column using CH2Cl2 as eluent. After condensation, 1.21 g of an orange solid is obtained (51%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06413655B2uspto-grants-2002_07