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Dimethylformamide → HCID 13259295, 화합물

HRID 436413
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HRID 436413 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:13]3[N:14]=[CH:15][CH:16]=[CH:17][C:12]=3[CH2:11][NH:10][C:9]2=[O:18])[CH:5]=[CH:6][CH:7]=1.[CH3:19]N(C)C=O.[H-].[Na+].FCOS([O-])(=O)=O>O>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:13]3[N:14]=[CH:15][CH:16]=[CH:17][C:12]=3[CH2:11][N:10]([CH3:19])[C:9]2=[O:18])[CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 132592941-(3-Chlorophenyl)-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-oneHCID 21452456HCID 21452456, 화합물

생성물 1

HCID 13259295HCID 13259295, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 2.6 g of 1-(m-chlorophenyl)-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine and 20 ml of dimethylformamide was added 0.6 g of sodium hydride and the mixture was stirred for 15 minutes. To this was further added 3.4 g of fluoromethylsulfate, and stirring was continued for 1.5 hours at room temperature. After the reaction was finished, the solvent was distilled off from the resulting mixture under reduced pressure. The residue thus obtained was diluted with water, extracted with ether and dehydrated. The ether solution was applied on a column of alumina, and then eluted with ether. The ether was evaporated from the eluate, and the residue was recrystallized from a mixture of ether and petroleum ether to give 2.1 g of 1-(m-chlorophenyl)-3-methyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine as colorless prisms, melting at 139° - 140° C.

후처리

  1. stirringstirring
  2. waitwas continued for 1.5 hours at room temperature
  3. distillationthe solvent was distilled off from the resulting mixture under reduced pressure
  4. customThe residue thus obtained
  5. extractionextracted with ether
  6. washeluted with ether
  7. customThe ether was evaporated from the eluate, and the residue
  8. customwas recrystallized from a mixture of ether and petroleum ether

출처 및 근거

ORD 기록
ord-be2a340c10dc4a89bcfe1d115e638aab
출처 데이터셋
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04009166

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