Phenyl thioxochloroformate → 2-Isothiocyanato-4,6-dimethoxypyrimidine
反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([NH:11][Si](C)(C)C)[N:4]=1.C1C=CC(O[C:23](Cl)=[S:24])=CC=1>C(#N)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([N:11]=[C:23]=[S:24])[N:4]=1参加物
4
実験手順
A solution of 45.0 g of 4,6-dimethoxy-2-trimethylsilylaminopyrimidine and 35.0 g of phenyl chlorothionocarbonate in 300 ml of acetonitrile is refluxed for 10 hours. The reaction solution is concentrated under reduced pressure to remove acetonitrile. Toluene (300 ml) is added to the residue and filtered to remove insoluble substance. The filtrate is concentrated under reduced pressure and purified by silica gel column-chromatography (eluent: ethyl acetate:hexane =1:1). 4,6-Dimethoxy-2-isothiocyanatopyrimidine (17.0 g) is obtained from the first eluate. mp 85°~86° C.
後処理
- concentrationThe reaction solution is concentrated under reduced pressure
- customto remove acetonitrile
- additionToluene (300 ml) is added to the residue
- filtrationfiltered
- customto remove insoluble substance
- concentrationThe filtrate is concentrated under reduced pressure
- custompurified by silica gel column-chromatography (eluent: ethyl acetate:hexane =1:1)
出典と根拠
- ORDレコード
- ord-af1813f5d4054331afb5433f76507d3a
- 出典データセット
- uspto-grants-1990_01
- 特許番号
- US04897105
反応ノート
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