Sodium Bicarbonate → HCID 71433889, 화합물

HRID 969733

반응식

HRID 969733 반응식
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

참가 물질

6

반응물 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)

생성물 1

HCID 71433889HCID 71433889, 화합물수율 92.5%

시약·촉매·용매 2

HCID 4875Potassium Iodide촉매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d736e404b79343de9a0344cdbc43413e
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07307168B2

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