Cesium carbonate → HCID 118194484, 화합물

HRID 633701

반응식

HRID 633701 반응식
[Cl:1][C:2]1[N:3]=[C:4]2[NH:12][C@H:11]([C:13]([F:16])([F:15])[F:14])[CH2:10][CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1.C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:24][C:25]([C:27]1[C:28]([CH3:33])=[N:29][O:30][C:31]=1[CH3:32])=[O:26]>C(#N)C>[Cl:1][C:2]1[N:3]=[C:4]2[N:12]([CH2:24][C:25]([C:27]3[C:28]([CH3:33])=[N:29][O:30][C:31]=3[CH3:32])=[O:26])[C@H:11]([C:13]([F:14])([F:15])[F:16])[CH2:10][CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 889959652-Bromo-1-(3,5-dimethyl-4-isoxazolyl)ethanoneHCID 136238740(S)-8-chloro-2-(trifluoromethyl)-3,4-dihydro-1H-pyrimido[1,2-a]pyrimidin-6(2H)-one

생성물 1

HCID 118194484HCID 118194484, 화합물수율 99.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A suspension of 150 mg (0.591 mmol) of (8S)-2-chloro-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one and 578.13 mg (1.77 mmol) of cesium carbonate in 10 mL of acetonitrile is stirred for 15 minutes at room temperature. 154.76 mg (0.709 mmol) of 2-bromo-1-(3,5-dimethylisoxazol-4-yl)ethanone are then added. After stirring overnight at room temperature, the reaction mixture is evaporated and the residue is taken up in water and extracted with ethyl acetate. The organic phase is dried over magnesium sulfate and evaporated to dryness to give 230 mg of (8S)-2-chloro-9-[2-(3,5-dimethylisoxazol-4-yl)-2-oxoethyl]-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one, corresponding to the following characteristics:

후처리

  1. stirringAfter stirring overnight at room temperature
  2. customthe reaction mixture is evaporated
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-1eb759f247c542f498111763d19012a4
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321790B2

연결된 노트

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