参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | 氢化钠 | HCID 24758 | — |
| 反应物 | 4-叔丁基苯乙醇 | HCID 79410 | — |
| 反应物 | 4-Chloro-5-methoxy-6-(methoxymethyl)pyrimidine | HCID 15279350 | — |
| 反应物 | HCID 178418361 | HCID 178418361 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 溶剂 | Water methylene chloride | HCID 21908982 | — |
| 产物 | 4-[2-(4-Tert-butylphenyl)ethoxy]-5-methoxy-6-methoxymethylpyrimidine | HCID 67839148 | 46% |
反应步骤
5.4 g (0.03 mol) of 2-(4-tert-butylphenyl)ethanol were added dropwise at 50° C. to a suspension of 1.2 g (0.03 mol) of sodium hydride (60% dispersion in oil) in 50 ml of dry dimethylformamide, and the mixture was stirred until the evolution of hydrogen had ceased. The mixture was cooled to 0° C., and 4.7 g (0.025 mol) of 4-chloro-5-methoxy-6-methoxymethylpyrimidine (Coll. Czechoslov. Chem. Commun. 33, 2266 (1968)) were added. The mixture was stirred for 1 hour at room temperature and for 2 hours at 100° C. After the solvent had been stripped off, the residue was taken up in dichloromethane/water, and the organic phase was dried and evaporated on a rotary evaporator. The crude product was chromatographed on silica gel using ethyl acetate. 3.8 g (46% of theory) of 4-[2-(4-tert-butylphenyl)ethoxy]-5 -methoxy-6 -methoxymethylpyrimidine were obtained in the form of a yellow oil.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US05859020 |
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| 来源数据集 | uspto-grants-1999_01 |
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| ORD ID | ord-5f15bb1b4b234011ac016c5a9a64901d |
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| 来源说明 | uspto-grants-1999_01 |
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