関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 1,3-Dimethyladamantane | HCID 12800 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(3,5-Dimethyltricyclo(3.3.1.13,7)dec-1-yl)formamide | HCID 2842768 | 89.3% |
反応手順
In sequence, 4 mL 65% technical nitric acid and then within three hours 50 mL 98% technical sulfuric acid are added to 6.572 g (40 mmol) 1,3-dimethyladamantane at 0° C. It is stirred over night at 0° C. and the mixture is poured at 0° C. onto 100 mL formamide in a round bottom flask which is provided with a drying tube. This mixture is stirred for 30 min at 0° C. and for 90 min at room temperature and 200 mL dichloromethane and 200 mL water are added. After phase separation, the organic phase is washed with water and 2% NaHCO3-solution, is dried, over Na2SO4 and is freed from solvents at the rotary evaporator. The remaining oil is chromatographically purified (SiO2, CHCl3/acetone (20:1), Rf=0.39). 7.41 g (89.3%) of the formamide are obtained as a nearly colourless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08138375B2 |
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| 出典データセット | uspto-grants-2012_03 |
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| ORD ID | ord-723f5263104f4e40966cfdeb7d64ed1c |
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| 出典メモ | uspto-grants-2012_03 |
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