Water → [6-(2-Methoxy-phenyl)-pyrimidin-4-yl]-carbamic acid ethyl ester

HRID 1020070

反応式

HRID 1020070 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH2:15])[CH:10]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:23][CH2:24][O:25][CH:26]=[O:27].O>CC(=O)CC>[CH2:24]([O:25][C:26](=[O:27])[NH:15][C:11]1[CH:10]=[C:9]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[O:2][CH3:1])[N:14]=[CH:13][N:12]=1)[CH3:23]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 2467482-Chloroethyl formateHCID 49758439HCID 49758439、化合物

生成物 1

HCID 59509103[6-(2-Methoxy-phenyl)-pyrimidin-4-yl]-carbamic acid ethyl ester収率 44.8%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 6-(2-methoxy-phenyl)-pyrimidin-4-ylamine (XXIV) (1.0 g, 4.9 mmol) and potassium carbonate (4.0 g, 29 mmol) in 2-butanone (10 ml), chloroethylformate (0.50 ml, 4.9 mmol) was added and the mixture was refluxed for 3 hours at 80° C. The reaction was monitored by TLC. After completion of the reaction, water was added and the mixture was extracted with ethyl acetate. The organic layer was separated, dried over anhydrous sodium sulfate and concentrated to provide 0.60 g of [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-carbamic acid ethyl ester (XL).

後処理

  1. additionwas added
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-df3a111454854ef9aba1f62402650947
出典データセット
uspto-grants-2014_05
特許番号
US08716296B2

関連ノート

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