2-Amino-4,6-dimethoxypyrimidine → Ethoxysulfuron

HRID 1030007ノート

反応式

HRID 1030007 の反応式
[CH2:1]([O:3][C:4]1[CH:16]=[CH:15][CH:14]=[CH:13][C:5]=1[O:6][S:7]([N:10]=[C:11]=[O:12])(=[O:9])=[O:8])[CH3:2].[NH2:17][C:18]1[N:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH3:27])[N:19]=1>ClCCl>[CH3:27][O:26][C:20]1[CH:21]=[C:22]([O:24][CH3:25])[N:23]=[C:18]([NH:17][C:11](=[O:12])[NH:10][S:7]([O:6][C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[O:3][CH2:1][CH3:2])(=[O:9])=[O:8])[N:19]=1

参加物

4

反応物 2

HCID 1189462-Amino-4,6-dimethoxypyrimidineHCID 190299582-Ethoxyphenoxysulfonyl isocyanate

生成物 1

HCID 3623881Ethoxysulfuron収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

A solution of 97.2 g (0.4 mol) of the product of Example 1 in 100 ml of dichloromethane is added dropwise at 25° C. to 62.0 g (0.4 mol) of 2-amino-4,6-dimethoxypyrimidine in 600 ml of dichloromethane. Stirring at room temperature is continued for 16 hours, the mixture is diluted with 600 ml of dichloromethane, and the organic phase is washed twice with 500 ml portions of 2N hydrochloric acid and once with 500 ml of water. After the mixture has been dried using sodium sulfate and after the solvent has been removed on a rotary evaporator, an oily product remains which crystallizes on trituration with diethyl ether. 145.0 g (91% of theory) of 3-(4,6-dimethoxypyrimidin-2-yl)-1-(2-ethoxyphenoxysulfonyl)urea of melting point 145°-147° C. are obtained.

後処理

  1. washthe organic phase is washed twice with 500 ml portions of 2N hydrochloric acid and once with 500 ml of water
  2. customAfter the mixture has been dried
  3. customafter the solvent has been removed on a rotary evaporator
  4. customcrystallizes on trituration with diethyl ether

出典と根拠

ORDレコード
ord-71216268f7ae429fa7aaf10033747492
出典データセット
uspto-grants-1992_04
特許番号
US05104443

反応ノート

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