関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Chloro-4-nitrophenol | HCID 10283 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Chloro-2-methylthiopyrimidine | HCID 97113 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Methylsulfanyl-4-(3-chloro-4-nitrophenoxy)-pyrimidine | HCID 67523947 | 64.1% |
反応手順
160 mg (6.34 mmol) 95% sodium hydride was given to a solution of 1.00 g (5.76 mmol) 3-chloro-4-nitrophenol in 15 ml DMF. Stirring was continued for 30 min. at room temperature. 925 mg (5.76 mmol) 4-chloro-2-methylsulfanyl-pyrimidine was added and the mixture heated to 80° C. for 16 h. The reaction mixture was evaporated, taken up with water and extracted with ethyl acetate. The organic phase was extracted with water, dried (sodium sulphate) and evaporated. The obtained material was dissolved in ethyl acetate and purified by chromatography over silica (ethyl acetate/n-heptane) to give 1.10 g (64%) 4-(3-chloro-4-nitro-phenoxy)-2-methylsulfanyl-pyrimidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08080552B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-33c7b7ddca184643b13bb176aaa90e9f |
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| 出典メモ | uspto-grants-2011_12 |
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