Hydrochloric Acid → HCID 15023844, 화합물

HRID 1461033노트

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HRID 1461033 반응식
[CH:1]1([NH:4][CH:5]=[C:6]([C:12](=[O:27])[C:13]2[C:18]([NH2:19])=[C:17]([F:20])[C:16]([F:21])=[C:15]([O:22][CH:23]([F:25])[F:24])[C:14]=2F)[C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:3][CH2:2]1.[H-].[Na+].Cl>O1CCCC1>[NH2:19][C:18]1[C:17]([F:20])=[C:16]([F:21])[C:15]([O:22][CH:23]([F:25])[F:24])=[C:14]2[C:13]=1[C:12](=[O:27])[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:5][N:4]2[CH:1]1[CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 178471897ethyl 2-[2-amino-5-(difluoromethoxy)-3,4,6-trifluorobenzoyl]-3-(cyclopropylamino)prop-2-enoate

생성물 1

HCID 15023844HCID 15023844, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The whole of the ethyl 3-cyclopropylamino-2-(6-amino-3-difluoromethoxy-2,4,5-trifluorobenzoyl)acrylate prepared as described above was dissolved in 340 ml of tetrahydrofuran, and 3.82 g (0.096 mole) of a 60% w/w dispersion of sodium hydride in mineral oil were added slowly to the resulting solution, whilst ice-cooling. The mixture was then stirred at the same temperature for 30 minutes, and then at room temperature for a further 1 hour. At the end of this time, the reaction mixture was acidified by the addition of 96 ml of 1N aqueous hydrochloric acid, whilst stirring vigorously. The resulting precipitate was collected by filtration and washed with water and with ethanol, in that order, to give 18.76 g of ethyl 5-amino-1-cyclopropyl-8-difluoromethoxy-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate [(XXII), R1 =--OCHF2, R17 =C2H5, X=F] as a colorless powder, melting at 295°-296° C.

후처리

  1. temperaturecooling
  2. waitat room temperature for a further 1 hour
  3. stirringwhilst stirring vigorously
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water and with ethanol, in that order

출처 및 근거

ORD 기록
ord-4647239a93664c3d8df5f7012919f215
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05073556

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