Phenyl thioxochloroformate → 2-Isothiocyanato-4-methoxy-6-methylpyrimidine
反応式
[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]参加物
4
反応条件
- 温度
- 80 °C
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-09ed0ef466724d298214983b1f0b370d
- 出典データセット
- uspto-grants-1990_01
- 特許番号
- US04897105
反応ノート
読み込み中…