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Triethylamine → 3-Ethoxycarbonyl-7,8-difluoro-1-methoxy-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine

HRID 1073596
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인쇄 미리보기

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HRID 1073596 반응식
C(N(CC)CC)C.Cl.[O:9]([NH2:11])[CH3:10].Cl[C:13]1[C:22]([C:23]([C:25](=[CH:31]N(C)C)[C:26]([O:28][CH2:29][CH3:30])=[O:27])=[O:24])=[CH:21][C:20]2[C:15](=[CH:16][C:17]([F:36])=[C:18]([F:35])[CH:19]=2)[N:14]=1>ClC(Cl)Cl>[CH2:29]([O:28][C:26]([C:25]1[C:23](=[O:24])[C:22]2[CH:21]=[C:20]3[CH:19]=[C:18]([F:35])[C:17]([F:36])=[CH:16][C:15]3=[N:14][C:13]=2[N:11]([O:9][CH3:10])[CH:31]=1)=[O:27])[CH3:30]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 53731972Ethyl 2-(2-chloro-6,7-difluoroquinoline-3-carbonyl)-3-dimethylaminoacrylate

생성물 1

HCID 148533423-Ethoxycarbonyl-7,8-difluoro-1-methoxy-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine수율 79.8%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
20 °C

실험 절차

2.13 g of triethylamine are added to a suspension of 1.7 g of methoxylamine hydrochloride in 40 cm3 of trichloromethane. After stirring for 15 minutes at a temperature close to 20° C., 3.69 g of ethyl 2-(2-chloro-6,7-difluoroquinoline-3-carbonyl)-3-dimethylaminoacrylate are added to the solution obtained and the mixture is stirred for 4 hours and a half at about 20° C. The reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at a temperature close to 50° C. The residue is taken up in 70 cm3 of ethanol and 3.6 g of triethylamine and the mixture is heated for 30 minutes at a temperature close to 75° C. After cooling to about 20° C., the precipitate obtained is drained and washed with 3 times 30 cm3 of ethanol. 2.67 g of 3-ethoxycarbonyl-7,8-difluoro-1-methoxy-4-oxo-1,4-dihydro-benzo [b][1,8]naphthyridine are obtained in the form of a pale yellow solid melting at 266°-268° C.

후처리

  1. customclose to 20° C.
  2. customobtained
  3. stirringthe mixture is stirred for 4 hours
  4. customat about 20° C
  5. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at a temperature
  6. customclose to 50° C
  7. temperature3.6 g of triethylamine and the mixture is heated for 30 minutes at a temperature
  8. customclose to 75° C
  9. customthe precipitate obtained
  10. washwashed with 3 times 30 cm3 of ethanol

출처 및 근거

ORD 기록
ord-cae6fe1a7e7040908a95edda2abd61ae
출처 데이터셋
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04970213

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