Hydrochloric Acid → 8-Chloro-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid

HRID 344846

반응식

HRID 344846 반응식
[Cl:1][C:2]1[C:3]([F:23])=[CH:4][C:5]2[C:6]([CH:22]=1)=[N:7][C:8]1[N:9]([CH3:21])[CH:10]=[C:11]([C:16]([O:18]CC)=[O:17])[C:12](=[O:15])[C:13]=1[CH:14]=2.Cl>C(O)(=O)C>[Cl:1][C:2]1[C:3]([F:23])=[CH:4][C:5]2[C:6]([CH:22]=1)=[N:7][C:8]1[N:9]([CH3:21])[CH:10]=[C:11]([C:16]([OH:18])=[O:17])[C:12](=[O:15])[C:13]=1[CH:14]=2

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 147005498-Chloro-3-ethoxycarbonyl-7-fluoro-1-methyl-4-oxo-1,4-dihydro-benzo[b][1,8]naphthyridine

생성물 1

HCID 147005548-Chloro-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid수율 92.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

A suspension of 8-chloro-3-ethoxycarbonyl-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]-naphthyridine (15 g) in acetic acid (150 cc) and 17.5% strength aqueous hydrochloric acid solution (150 cc) is heated to a temperature in the region of 100° C. with stirring for 4 hours. After cooling to a temperature in the region of 20° C., the product is drained, washed with water (2×100 cc) and washed with ethanol (2×150 cc) and then ethyl ether (2×100 cc). 8-Chloro-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid (12.7 g) is obtained in the form of a beige solid, subliming at 400°-405° C., which is used without further purification for the subsequent steps.

후처리

  1. temperatureAfter cooling to a temperature in the region of 20° C.
  2. washwashed with water (2×100 cc)
  3. washwashed with ethanol (2×150 cc)

출처 및 근거

ORD 기록
ord-2742418d14ba4f89a1e7f076e3f66b8b
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05053509

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