反応 #736792

ord-d00e77a6b43a4d8a92c85b1e35d241b5

反応方程式

Cn1c(=O)c(C#N)c2c3c(c(Br)ccc31)C(=O)c1ccccc1-2
6-bromo-1-cyano-3-methyl-3H-dibenz[f,ij]isoquinoline-2,7-dione
CC(O)c1ccc(N)cc1
p-aminophenylethanol
CC(=O)[O-].[K+]
potassium acetate
Cl
HCl
Cn1c(=O)c(C#N)c2c3c(c(Nc4ccc(CCO)cc4)ccc31)C(=O)c1ccccc1-2
1-Cyano-6-[4-(2-Hydroxyethyl)Anilino]-3-Methyl-3H-Dibenzo[f,ij]Isoquinoline-2,7-Dione

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The solid product was collected by filtration
  2. 2
    洗浄washed with water
  3. 3
    その他dried in air
  4. 4
    その他recrystallized twice from nitrobenzene
  5. 5
    その他to remove a red impurity and traces of starting material
  6. 6
    その他was obtained

実験手順

A mixture of 6-bromo-1-cyano-3-methyl-3H-dibenz[f,ij]isoquinoline-2,7-dione (2.0 g), p-aminophenylethanol (15 g), potassium acetate (2.0 g), a trace of cupric acetate, and butanol (10 ml) was heated gradually to about 80° C., held for 5-10 minutes, and then drained into 250 ml of 10% HCl. The solid product was collected by filtration, washed with water, dried in air, and recrystallized twice from nitrobenzene to remove a red impurity and traces of starting material. A yield of 0.65 g of product, which had a visible absorption maximum at 587 nm in acetone, was obtained, thus imparting a reddish-blue color to acetone. The structure is as follows: ##STR6##

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04740581uspto-grants-1988_04