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

HRID 326975노트

반응식

HRID 326975 반응식
[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

참가 물질

4

반응물 2

HCID 1189462-Amino-4,6-dimethoxypyrimidineHCID 14722020HCID 14722020, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f9313004172b46c28d858673f32a89cd
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05272129

반응 노트

불러오는 중…