Dabco → 1-(1-Fluoromethyl-1-methyl-2-fluoroethyl)-6-fluoro-7-[(1S,6R)-2-oxa-5,8-diazabicyclo[4.3.0]non-8-yl]-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid

HRID 2302232ノート

反応式

HRID 2302232 の反応式
[F:1][CH2:2][C:3]([N:7]1[C:16]2[C:11](=[CH:12][C:13]([F:18])=[C:14](F)[CH:15]=2)[C:10](=[O:19])[C:9]([C:20]([OH:22])=[O:21])=[CH:8]1)([CH3:6])[CH2:4][F:5].[C@H:23]12[CH2:31][NH:30][CH2:29][C@H:28]1[NH:27][CH2:26][CH2:25][O:24]2.N12CCN(CC1)CC2>C(#N)C>[F:1][CH2:2][C:3]([N:7]1[C:16]2[C:11](=[CH:12][C:13]([F:18])=[C:14]([N:30]3[CH2:31][C@H:23]4[C@H:28]([NH:27][CH2:26][CH2:25][O:24]4)[CH2:29]3)[CH:15]=2)[C:10](=[O:19])[C:9]([C:20]([OH:22])=[O:21])=[CH:8]1)([CH3:6])[CH2:4][F:5]

参加物

5

反応物 3

HCID 9237DabcoHCID 18459849HCID 18459849、化合物HCID 55287490Rac-(4ar,7as)-octahydropyrrolo[3,4-b]morpholine

生成物 1

HCID 540502771-(1-Fluoromethyl-1-methyl-2-fluoroethyl)-6-fluoro-7-[(1S,6R)-2-oxa-5,8-diazabicyclo[4.3.0]non-8-yl]-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 1-(1-fluoromethyl-1-methyl-2-fluoroethyl)-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (400 mg, 1.26 mmol), (1S,6R)-2-oxa-5,8-diazabicyclo[4.3.0]nonane (176 mg, 1.39 mmol) and 1,4-diazabicyclo[2.2.2]octane (141 mg, 1.26 mmol) in absol. acetonitrile (20 ml) is heated under reflux overnight. After cooling the reaction mixture to room temperature, the precipitated crystals are filtered off and washed with acetonitrile.

後処理

  1. temperatureunder reflux overnight
  2. filtrationthe precipitated crystals are filtered off
  3. washwashed with acetonitrile

出典と根拠

ORDレコード
ord-4ffc6aeec65648a59e63338a164e6077
出典データセット
uspto-grants-2002_08
特許番号
US06432948B1

反応ノート

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