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Phenyl thioxochloroformate → 2-Isothiocyanato-4,6-dimethoxypyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenyl thioxochloroformate | HCID 70498 | — |
| 反応物 | 4,6-Dimethoxy-N-(trimethylsilyl)pyrimidin-2-amine | HCID 19868312 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Isothiocyanato-4,6-dimethoxypyrimidine | HCID 14253942 | 43.5% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04897105 |
| 出典データセット | uspto-grants-1990_01 |
| ORD ID | ord-af1813f5d4054331afb5433f76507d3a |
| 出典メモ | uspto-grants-1990_01 |