تفاعل #69686

ord-26a2cbfbb4d34563afa8982f03fdf0ef

معادلة التفاعل

O=C1OC(=O)c2c(O)cccc21
3-hydroxyphthalic anhydride
COc1ccc(CN)cc1
4-methoxybenzylamine
CC(=O)O
acetic acid
COc1ccc(CN2C(=O)c3cccc(O)c3C2=O)cc1
title compound
المردود 81.1%
COc1ccc(CN2C(=O)c3cccc(O)c3C2=O)cc1
Hydroxy-2-(4-methoxy-benzyl)-isoindole-1,3-dione
المردود 81.1%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto cool
  2. 2
    ترشيحThe white solid was collected by filtration
  3. 3
    غسيلwashed well with water
  4. 4
    أخرىdried

الإجراء التجريبي

A mixture of 3-hydroxyphthalic anhydride (543 mg, 3.31 mmol), 4-methoxybenzylamine (0.43 mL, 3.31 mmol) and acetic acid (3 mL) was heated at 100° C. for 4 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 (760 mg, 81%). 1H NMR (DMSO-d6) 11.03 (1H, s), 7.61 (1H, dd), 7.28 (1H, d), 7.23-7.19 (3H, m), 6.89-6.86 (2H, m), 4.63 (2H, s), 3.71 (3H, s). MS: [M−H+] 282.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08530469B2uspto-grants-2013_09