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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 20071620, 화합물 → HCID 20071612, 화합물

HRID 981203
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HRID 981203 반응식
[Cl:1][C:2]1[C:3]([F:26])=[CH:4][C:5]2[C:6]([CH:25]=1)=[N:7][C:8]1[N:9]([CH2:21][O:22][CH2:23][CH3:24])[CH:10]=[C:11]([C:16]([O:18]CC)=[O:17])[C:12](=[O:15])[C:13]=1[CH:14]=2>O.C(O)C.[OH-].[K+]>[Cl:1][C:2]1[C:3]([F:26])=[CH:4][C:5]2[C:6]([CH:25]=1)=[N:7][C:8]1[N:9]([CH2:21][O:22][CH2:23][CH3:24])[CH:10]=[C:11]([C:16]([OH:18])=[O:17])[C:12](=[O:15])[C:13]=1[CH:14]=2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 20071620HCID 20071620, 화합물

생성물 1

HCID 20071612HCID 20071612, 화합물수율 72%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 14797Potassium Hydroxide용매

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온도
20 °C

실험 절차

A suspension of 6 g of 8-chloro-3-ethoxycarbonyl-1-ethoxymethyl-7-fluoro-4-oxo-1,4-dihydro-benzo[b][1,8]naphthyridine in 120 cm3 of water, 120 cm3 of ethanol and 47.5 cm3 of 2N aqueous potassium hydroxide solution is heated, with stirring, at a temperature close to 75° C. for 2 hours and a half. A small amount of insoluble matter is removed by filtering at the same temperature. After cooling to about 20° C., 6 cm3 of acetic acid are added to the filtrate. The precipitate obtained is drained, washed with 3 times 20 cm3 of water and recrystallized from 60 cm3 of dimethylformamide. 4 g of 8-chloro-1-ethoxymethyl-7-fluoro-4-oxo-1,4-dihydro-benzo[b][1,8]naphthyridine-3-carboxylic acid are obtained in the form of a yellow solid which decomposes at 285° C.

후처리

  1. temperatureis heated
  2. customclose to 75° C. for 2 hours
  3. customA small amount of insoluble matter is removed
  4. filtrationby filtering at the same temperature
  5. addition6 cm3 of acetic acid are added to the filtrate
  6. customThe precipitate obtained
  7. washwashed with 3 times 20 cm3 of water
  8. customrecrystallized from 60 cm3 of dimethylformamide

출처 및 근거

ORD 기록
ord-6c70d4a6a1ab4b46a7ee28010608bc04
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04990515

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