関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Acetylacetone | HCID 31261 | — |
| 反応物 | Morpholine-4-carboximidamide Hydrobromide | HCID 2806564 | — |
| 生成物 | 4-(4,6-Dimethylpyrimidin-2-yl)morpholine | HCID 676802 | 90% |
反応手順
To a suspension of morpholinoformamidine hydrobromide (2.0 g, 9.52 mmol) in ethanol (6 ml) potassium tert-butoxide (1.068 g, 9.52 mmol) then acetylacetone (2 ml, 20 mmol) were added. The reaction mixture was flashed with argon, sealed in the Emrys process vial and heated under microwave irradiation at 140° C. for 5 min. After cooling it was quenched with ethyl acetate (50 ml), filtered via plug of SiO2 (5 g) and eluted with ethyl acetate. Volatiles were removed in vacuo at 70° C. to furnish 1.65 g of pale brown oil that solidified overnight. Yield 90%. LC-MS (m/z) 193.9 (MH+); tR=0.71. 1H NMR (500 MHz, DMSO-d6): 2.23 (s, 6H), 3.62 (m, 4H), 3.67 (m, 4H), 6.44 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07683058B2 |
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| 出典データセット | uspto-grants-2010_03 |
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| ORD ID | ord-93561c729c284735bcad2c693e0a3499 |
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| 出典メモ | uspto-grants-2010_03 |
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