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

HRID 1694732

反応式

HRID 1694732 の反応式
[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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 74508Pyrimidine, 2,4-dichloro-5-methyl-HCID 178486264HCID 178486264、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-86007e06b1a2473aa58df9d9b94b2f1b
出典データセット
uspto-grants-2012_04
特許番号
US08158820B2

関連ノート

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