Water → 1-Cyclopropyl-6,8-difluoro-7-[7-ethyl-3,7-diazabicyclo [3.3.0] oct-1(5)-en-3-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

HRID 1534827노트

반응식

HRID 1534827 반응식
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:23])=[C:11]([N:15]4[CH2:22][C:21]5[CH2:20][NH:19][CH2:18][C:17]=5[CH2:16]4)[C:12]=3[F:14])[C:7](=[O:24])[C:6]([C:25]([OH:27])=[O:26])=[CH:5]2)[CH2:3][CH2:2]1.[CH2:28](I)[CH3:29].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:23])=[C:11]([N:15]4[CH2:22][C:21]5[CH2:20][N:19]([CH2:28][CH3:29])[CH2:18][C:17]=5[CH2:16]4)[C:12]=3[F:14])[C:7](=[O:24])[C:6]([C:25]([OH:27])=[O:26])=[CH:5]2)[CH2:2][CH2:3]1

참가 물질

6

반응물 4

HCID 962WaterHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 98643051-Cyclopropyl-7-[3,7-diazabicyclo[3.3.0]oct-1(5)-en-3-yl]-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

생성물 1

HCID 199082411-Cyclopropyl-6,8-difluoro-7-[7-ethyl-3,7-diazabicyclo [3.3.0] oct-1(5)-en-3-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid수율 52.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1-cyclopropyl 6,8-difluoro-7-[3,7-diazabicyclo [3.3.0]-oct-1(5)-en-3-yl]-1,4-dihydro-4-oxoquinoline-3-carboxyl-ic acid (0.37 g) in dimethyl formamide (30 ml), which was prepared in Example 11, ethyliodide (0.17 g) and potassium carbonate (powder, 1 g) were added and stirred at room temperature for 24 hours. To the reaction mixture, water (100 ml) was added and the precipitate was filtered. The filter cake was purified by silica gel column chromatography (CHCl3 :methanol:acetic acid=6:3:1) to give the title compound (0.21 g, yield 52%).

후처리

  1. additionwere added
  2. filtrationthe precipitate was filtered
  3. customThe filter cake was purified by silica gel column chromatography (CHCl3 :methanol:acetic acid=6:3:1)

출처 및 근거

ORD 기록
ord-0d943c4d32f74101b46bc6db8669c410
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05091384

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