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 1534827ノート

反応式

HRID 1534827 の反応式
[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

参加物

6

反応物 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

生成物 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 acid収率 52.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-0d943c4d32f74101b46bc6db8669c410
出典データセット
uspto-grants-1992_02
特許番号
US05091384

反応ノート

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