Sodium Bicarbonate → 5-Chloro-6-{4-[2-chloro-6-(4-fluoro-phenyl)-pyrimidin-4-yl]piperazin-1-yl}-nicotinic acid ethyl ester

HRID 1444102ノート

反応式

HRID 1444102 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=2)[N:3]=1.C([O-])(O)=O.[Na+].[CH2:21]([O:23][C:24](=[O:38])[C:25]1[CH:30]=[C:29]([Cl:31])[C:28]([N:32]2[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]2)=[N:27][CH:26]=1)[CH3:22]>CCO>[CH2:21]([O:23][C:24](=[O:38])[C:25]1[CH:30]=[C:29]([Cl:31])[C:28]([N:32]2[CH2:37][CH2:36][N:35]([C:6]3[CH:5]=[C:4]([C:9]4[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=4)[N:3]=[C:2]([Cl:1])[N:7]=3)[CH2:34][CH2:33]2)=[N:27][CH:26]=1)[CH3:22]

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 116373222,4-Dichloro-6-(4-fluorophenyl)pyrimidineHCID 22028944Ethyl 5-chloro-6-(piperazin-1-YL)nicotinate

生成物 1

HCID 591683325-Chloro-6-{4-[2-chloro-6-(4-fluoro-phenyl)-pyrimidin-4-yl]piperazin-1-yl}-nicotinic acid ethyl ester

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of 2,4-dichloro-6-(4-fluoro-phenyl)-pyrimidine (2.82 g, 0.12 mol) and NaHCO3 (1.95 g, 0.023 mol) in EtOH at 0° C., add 5-chloro-6-piperazin-1-yl-nicotinic acid ethyl ester (3.44 g, 0.013 mol). Remove the ice bath and stir at room temperature for 16 h. Concentrate under reduced pressure and partition between EtOAc and brine. Dry the organic layer (Na2SO4) and concentrate under reduced pressure to give the title compound.

後処理

  1. customRemove the ice bath
  2. concentrationConcentrate under reduced pressure
  3. custompartition between EtOAc and brine
  4. dry with materialDry the organic layer (Na2SO4)
  5. concentrationconcentrate under reduced pressure

出典と根拠

ORDレコード
ord-563e5b1ee36541839db83f63b65e932d
出典データセット
uspto-grants-2010_02
特許番号
US07662830B2

反応ノート

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