Potassium Carbonate → N-(4-Chloro-5-methylpyrimidin-2-YL)-N-methylmethanesulfonamide

HRID 1694732

반응식

HRID 1694732 반응식
[CH3:1][NH:2][SH:3](=[O:5])=[O:4].Cl[C:7]1[N:12]=[C:11]([Cl:13])[C:10]([CH3:14])=[CH:9][N:8]=1.[C:15](=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:13][C:11]1[C:10]([CH3:14])=[CH:9][N:8]=[C:7]([N:2]([CH3:1])[S:3]([CH3:15])(=[O:5])=[O:4])[N:12]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 74508Pyrimidine, 2,4-dichloro-5-methyl-HCID 178486264HCID 178486264, 화합물

생성물 1

HCID 72211794N-(4-Chloro-5-methylpyrimidin-2-YL)-N-methylmethanesulfonamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of N-methylsulphonamide (3.35 g), 2,4-dichloro-5-methylpyrimidine (5 g) and potassium carbonate (4.3 g) in DMF (50 ml) was heated at 80° C. for 4 h. The reaction was quenched with water (200 ml) and extracted with ethylacetate. The organics were dried, evaporated under reduced pressure and the residue triturated with ether. The solid was filtered off (4-isomer) and the filtrate evaporated under reduced pressure and subjected to RPHPLC to obtain the 2-isomer, yield 0.37 g.

후처리

  1. customThe reaction was quenched with water (200 ml)
  2. extractionextracted with ethylacetate
  3. customThe organics were dried
  4. customevaporated under reduced pressure
  5. customthe residue triturated with ether
  6. filtrationThe solid was filtered off (4-isomer)
  7. customthe filtrate evaporated under reduced pressure
  8. customto obtain the 2-isomer, yield 0.37 g

출처 및 근거

ORD 기록
ord-86007e06b1a2473aa58df9d9b94b2f1b
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158820B2

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