反応 #2329044

ord-754c7b93dbbc4c6cbc822f5b8eff86d3

反応方程式

COc1ccc(C(=O)Cl)cc1
4-methoxy-benzoyl chloride
NNc1nnc(Cl)c2ccccc12
(4-chloro-phthalazin-1-yl)-hydrazine
NNc1nnc(Cl)c2ccccc12
compound C1
NNc1nnc(Cl)c2ccccc12
(4-chloro-phthalazin-1-yl)-hydrazine
COc1ccc(-c2nnc3c4ccccc4c(Cl)nn23)cc1
title compound
収率 54.3%
COc1ccc(-c2nnc3c4ccccc4c(Cl)nn23)cc1
6-Chloro-3-(4-methoxy-phenyl)-[1,2,4]triazolo[3,4-a]phthalazine
収率 54.3%

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled to ambient temperature
  2. 2
    ろ過filtered with suction
  3. 3
    洗浄rinsed with toluene
  4. 4
    その他The solid is recrystallized from N,N-dimethylformamide
  5. 5
    洗浄the precipitate is washed with water
  6. 6
    その他dried

実験手順

6.0 g (4-chloro-phthalazin-1-yl)-hydrazine (compound C1) are suspended in a mixture of 160 ml toluene and 18 ml triethylamine at 60° C. and treated with a solution of 6.0 g 4-methoxy-benzoyl chloride in 48 ml toluene. The mixture is stirred at 110° C. for 6 h, cooled to ambient temperature, filtered with suction and rinsed with toluene. The solid is recrystallized from N,N-dimethylformamide, the precipitate is washed with water and dried to yield 5.2 g of the title compound (m.p.: 192-193° C.).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07671050B2uspto-grants-2010_03