Potassium Carbonate → 6-Methyl-4-(1-Pyrrolidinylcarboxy)-2-Trichloromethylpyrimidine

HRID 66725

反応式

HRID 66725 の反応式
O[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]([Cl:12])([Cl:11])[Cl:10])[N:3]=1.[C:13](=[O:16])([O-])[O-:14].[K+].[K+].[N:19]1(C(Cl)=O)[CH2:23][CH2:22][CH2:21][CH2:20]1>CC(C)=O>[CH3:8][C:6]1[N:5]=[C:4]([C:9]([Cl:12])([Cl:11])[Cl:10])[N:3]=[C:2]([C:13]([O:14][N:19]2[CH2:23][CH2:22][CH2:21][CH2:20]2)=[O:16])[CH:7]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 709371-Pyrrolidinecarbonyl chlorideHCID 178429333HCID 178429333、化合物

生成物 1

HCID 545013486-Methyl-4-(1-Pyrrolidinylcarboxy)-2-Trichloromethylpyrimidine収率 125.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 5.8 g (0.027 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 3.3 g (0.024 mole) potassium carbonate, 3.2 g (0.024 mole) pyrrolidinecarbonyl chloride, and 100 ml acetone was refluxed 5.3 hours. A precipitate was filtered out and the filtrate rotary evaporated to give 9.8 g residue. This was taken up in chloroform, the solution washed with 1% sodium hydroxide, water, and dried over anhydrous magnesium sulfate. Rotary evaporation yielded 4.4 g residue which was recrystallized from petroleum ether to give 2.2 g (28% yield; mp 93°-95° C.) of product. The structure was confirmed via infrared and elemental analysis.

後処理

  1. temperaturewas refluxed 5.3 hours
  2. filtrationA precipitate was filtered out
  3. customthe filtrate rotary evaporated

出典と根拠

ORDレコード
ord-c92a06f657304b658322e781547f7510
出典データセット
uspto-grants-1982_08
特許番号
US04343803

関連ノート

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