2-Amino-4-chloro-6-methylpyrimidine → Methyl 2-[3-(4-chloro-6-methylpyrimidin-2-yl)-ureidosulfonyloxy]-3-methoxybenzoate

HRID 326976ノート

反応式

HRID 326976 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]([Cl:27])[CH:24]=[C:23]([CH3:28])[N:22]=1>C(Cl)Cl>[Cl:27][C:25]1[CH:24]=[C:23]([CH3:28])[N:22]=[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:26]=1

参加物

4

反応物 2

HCID 218102-Amino-4-chloro-6-methylpyrimidineHCID 14722020HCID 14722020、化合物

生成物 1

HCID 14722022Methyl 2-[3-(4-chloro-6-methylpyrimidin-2-yl)-ureidosulfonyloxy]-3-methoxybenzoate

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 2.9 g (0.02 mol) of 2-amino-4-chloro-6-methylpyrimidine 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 water. After drying with sodium sulfate and removing the solvent on a rotary evaporator, an oily product remains, which crystallizes on trituration with diisopropylether. 7.8 g (91% of theory of methyl 2-[3-(4-chloro-6-methylpyrimidin-2-yl)-ureidosulfonyloxy]-3-methoxybenzoate of melting point 140°-143° 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 diisopropylether

出典と根拠

ORDレコード
ord-47c771e9b6e5440d89b1866bf650543c
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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