2-Amino-4,6-dimethoxypyrimidine → Methyl 2-[3-(4,6-dimethoxypyrimidin-2-yl)-ureidosulfonyloxy]-3-methoxy-benzoate

HRID 326975ノート

反応式

HRID 326975 の反応式
[CH3:1][O:2][C:3](=[O:19])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([O:10][CH3:11])[C:5]=1[O:12][S:13]([N:16]=[C:17]=[O:18])(=[O:15])=[O:14].[NH2:20][C:21]1[N:26]=[C:25]([O:27][CH3:28])[CH:24]=[C:23]([O:29][CH3:30])[N:22]=1>C(Cl)Cl>[CH3:30][O:29][C:23]1[CH:24]=[C:25]([O:27][CH3:28])[N:26]=[C:21]([NH:20][C:17](=[O:18])[NH:16][S:13]([O:12][C:5]2[C:6]([O:10][CH3:11])=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([O:2][CH3:1])=[O:19])(=[O:15])=[O:14])[N:22]=1

参加物

4

反応物 2

HCID 1189462-Amino-4,6-dimethoxypyrimidineHCID 14722020HCID 14722020、化合物

生成物 1

HCID 14722021Methyl 2-[3-(4,6-dimethoxypyrimidin-2-yl)-ureidosulfonyloxy]-3-methoxy-benzoate収率 77%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
25 °C

実験手順

A solution of 5.4 g (0.02 mol) of the product from Example 1 in 10 ml of methylene chloride is added dropwise to 3.1 g (0.02 mol) of 2-amino-4,6-dimethoxypyrimidine in 50 ml of methylene chloride at 0° C. The mixture is subsequently stirred at 25° C. for 24 hours and diluted with 50 ml of methylene chloride and the organic phase is washed twice with 50 ml of 2N hydrochloric acid each time and once with 50 ml of water. After drying with sodium sulfate and removing the solvent on a rotary evaporator, an oily product remains, which crystallizes on trituration with diethylether. 6.8 g (77% of theory) of methyl 2-[3-(4,6-dimethoxypyrimidin-2-yl)-ureidosulfonyloxy]-3-methoxy-benzoate of melting point 169°-170° C. are obtained.

後処理

  1. washthe organic phase is washed twice with 50 ml of 2N hydrochloric acid each time
  2. dry with materialAfter drying with sodium sulfate
  3. customremoving the solvent
  4. customon a rotary evaporator
  5. customwhich crystallizes on trituration with diethylether

出典と根拠

ORDレコード
ord-f9313004172b46c28d858673f32a89cd
出典データセット
uspto-grants-1993_12
特許番号
US05272129

反応ノート

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