Sodium Bicarbonate → HCID 71433889、化合物

HRID 969733

反応式

HRID 969733 の反応式
Cl[CH2:2][CH2:3][C:4]1[C:9](=[O:10])[N:8]2[CH2:11][CH2:12][CH2:13][CH2:14][C:7]2=[N:6][C:5]=1[CH3:15].Cl.[F:17][C:18]1[CH:32]=[C:31]([F:33])[CH:30]=[CH:29][C:19]=1[C:20](=[N:27][OH:28])[CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.C(=O)([O-])O.[Na+]>C(#N)C.[I-].[K+]>[F:17][C:18]1[CH:32]=[C:31]([F:33])[CH:30]=[CH:29][C:19]=1[C:20](=[N:27][OH:28])[CH:21]1[CH2:26][CH2:25][N:24]([CH2:2][CH2:3][C:4]2[C:9](=[O:10])[N:8]3[CH2:11][CH2:12][CH2:13][CH2:14][C:7]3=[N:6][C:5]=2[CH3:15])[CH2:23][CH2:22]1

参加物

6

反応物 3

HCID 516892Sodium BicarbonateHCID 27630793-(2-Chloroethyl)-2-methyl-6,7,8,9-tetrahydro-4hpyrido(1,2-a)pyrimidin-4-oneHCID 57357481N-[(2,4-Difluorophenyl)(piperidin-4-yl)methylidene]hydroxylamine--hydrogen chloride (1/1)

生成物 1

HCID 71433889HCID 71433889、化合物収率 92.5%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide触媒HCID 6342Acetonitrile溶媒

実験手順

To a solution of 36.0 g (0.16 mole) of 3-(2-chloroethyl)-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one in 800 ml of acetonitrile 44.3 g of 4-(2,4-difluoro-benzoyl)-piperidine-oxime-hydrochloride, 33.6 g of sodium hydrogen carbonate and 0.66 g (4 millimoles) of potassium iodide are added. The reaction mixture is refluxed for 5 hours, cooled to room temperature and the solvent is removed in vacuo. The residue is taken up in 700 ml of water and extracted twice with 600 ml of dichloromethane each. The combined organic layers are dried over sodium sulfate and evaporated in vacuo. Thus 63.7 g of the title compound are obtained. Yield 92.5%. M.p.: 180-183° C.

後処理

  1. temperatureThe reaction mixture is refluxed for 5 hours
  2. customthe solvent is removed in vacuo
  3. extractionextracted twice with 600 ml of dichloromethane each
  4. dry with materialThe combined organic layers are dried over sodium sulfate
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-d736e404b79343de9a0344cdbc43413e
出典データセット
uspto-grants-2007_12
特許番号
US07307168B2

関連ノート

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