反応 #69687

ord-3204a4b7bfac4724a29b02172a4d9b12

反応方程式

O=C1OC(=O)c2c(O)cccc21
3-hydroxyphthalic anhydride
COc1ccc(CN)c(OC)c1
2,4-dimethoxybenzylamine
CC(=O)O
acetic acid
COc1ccc(CN2C(=O)c3cccc(O)c3C2=O)c(OC)c1
title compound
収率 73.0%
COc1ccc(CN2C(=O)c3cccc(O)c3C2=O)c(OC)c1
4-Hydroxy-2-(2,4-dimethoxy-benzyl)-isoindole-1,3-dione
収率 73.0%

溶媒

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool
  2. 2
    ろ過The white solid was collected by filtration
  3. 3
    洗浄washed well with water
  4. 4
    その他dried

実験手順

A mixture of 3-hydroxyphthalic anhydride (1.24 g, 7.6 mmol), 2,4-dimethoxybenzylamine (1.14 mL, 7.6 mmol) and acetic acid (5 mL) was heated at 80° C. for 24 hours. The mixture was allowed to cool and diluted with water (20 mL). The white solid was collected by filtration, washed well with water and dried to give the title compound (1.73 g, 73%). 1H NMR (DMSO-d6) 11.00 (1H, s), 7.62 (1H, dd), 7.29 (1H, d), 7.21 (1H, d), 6.90 (1H, d), 6.56 (1H, d), 6.43 (1H, dd), 4.59 (2H, s), 3.79 (3H, s), 3.72 (3H, s). MS: [M−H+] 314.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530469B2uspto-grants-2013_09