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HRID 344853作成日:2026年10月25日

Acetic Acid → HCID 53724661、化合物

https://huagongshe.com/reaction/344853

反応式

関与物質

役割名称HCID仕込み量
反応物Acetic AcidHCID 176—
反応物WaterHCID 962—
反応物2-(4-Fluorophenyl)piperazineHCID 4617623—
反応物8-Chloro-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acidHCID 14700554—
溶媒PyridineHCID 1049—
生成物HCID 53724661HCID 5372466146.8%

反応条件

温度115 °C

反応手順

A suspension of 8-chloro-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid (1.6 g) and (RS)-2-(4-fluorophenyl)piperazine (3.7 g) in pyridine (16 cc) is heated to a temperature in the region of 115° C. for 24 hours. The reaction mixture is concentrated under reduced pressure (20 kPa) at approximately 60° C. The residue is taken up with ethanol (40 cc) and concentrated again under reduced pressure under the above conditions. The solid obtained is taken up with water (10 cc), treated with 10% strength acetic acid (1.75 cc), drained and washed with water (2×10 cc) and ethanol (2×10 cc). After 2 recrystallizations in dimethylformamide (10 cc each time), (RS)-7-fluoro-8-[3-(4-fluorophenyl)-1-piperazinyl]-1-methyl-4-oxo-1,4-dihydrobenzo[b ][1,8]naphthyridine-3-carboxylic acid (1.1 g) is obtained in the form of a yellow solid, m.p. 270°-275° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05053509
出典データセットuspto-grants-1991_10
ORD IDord-86f51b4aa94f4fa0959685c631bcb861
出典メモuspto-grants-1991_10