Phenyl thioxochloroformate → 2-Isothiocyanato-4-methoxy-6-methylpyrimidine
반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[N:6]=[C:5]([NH:10][Si](C)(C)C)[N:4]=1.C1C=CC(O[C:22](Cl)=[S:23])=CC=1>C1(C)C=CC=CC=1>[N:10]([C:5]1[N:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([CH3:9])[N:6]=1)=[C:22]=[S:23]참가 물질
4
반응 조건
- 온도
- 80 °C
실험 절차
A mixture of 4.2 g of 4-methoxy-6-methyl-2-trimethylsilylaminopyrimidine and 3.5 g of phenyl chlorothionocarbonate in 30 ml of toluene is stirred with heating at ca. 80° C. for 5.5 hours. The reaction solution is cooled to room temperature and filtered to remove the precipitate. The filtrate is concentrated under reduced pressure, and the residue is purified by silica gel chromatography (eluent: ethyl acetate: toluene =1:3) to give the title compound (2.3 g). mp 54°~55° C.
후처리
- temperatureThe reaction solution is cooled to room temperature
- filtrationfiltered
- customto remove the precipitate
- concentrationThe filtrate is concentrated under reduced pressure
- customthe residue is purified by silica gel chromatography (eluent: ethyl acetate: toluene =1:3)
출처 및 근거
- ORD 기록
- ord-09ed0ef466724d298214983b1f0b370d
- 출처 데이터셋
- uspto-grants-1990_01
- 특허 번호
- US04897105
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