تفاعل #3254
ord-ce23a4c71bca4f4ba6dee847e17f8171
معادلة التفاعل
6-(((dimethylamino)ethyl)amino)-3-hydroxy-7H-indeno[2,1-c]quinoline-7-on
sulfuric acid
nitric acid
→
title compound
المردود 52.9%
6-(((dimethylamino)ethyl)amino)-3-hydroxy-4-nitro-7H-indeno[2,1-c]quinoline-7-on
المردود 52.9%
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىa crystal precipitated
- 2ترشيحwas collected by filtration
- 3أخرىThe crystal obtained
- 4أخرىwas purified by silica gel column chromatography (eluent
- 5أخرىa lower layer of chloroform:methanol:water=9:3:1(v/v/v)) and crystallized from ethanol-diethylether
الإجراء التجريبي
A mixture of 6-(((dimethylamino)ethyl)amino)-3-hydroxy-7H-indeno[2,1-c]quinoline-7-on obtained in example 3 (100 mg, 0.3 mmol), conc. sulfuric acid (1 ml) and nitric acid (1 ml) was stirred at 5° C. for 2 hours. The reaction mixture was poured into ice water, and a crystal precipitated was collected by filtration. The crystal obtained was purified by silica gel column chromatography (eluent; a lower layer of chloroform:methanol:water=9:3:1(v/v/v)) and crystallized from ethanol-diethylether to give 60 mg (yield: 52.9%) of title compound. The physicochemical properties thereof are shown in table 1.