関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Nitropropane | HCID 398 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Phenyl ethenesulfonate | HCID 564920 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Phenyl 3-methyl-3-nitrobutane-1-sulfonate | HCID 86616499 | — |
反応手順
A mixture of 9.43 g of phenyl ethenesulfonate and 4.60 ml of 2-nitro-propane was heated to 80° C. and, at 80° C., 0.89 ml of ethyidiisopropylamine was added dropwise. The mixture was stirred at 80° C. for 4 hours and 30 minutes, left to stand at RT for 16 hours and then stirred at 80° C. for a further 2 hours. Cooling to RT was followed by addition of 250 ml of a 2N aqueous HCl solution and extraction 3 times with 150 ml of EA each time. Drying over Na2SO4 and removal of the solvent in vacuo were followed by coevaporation 3 times with 100 ml of toluene each time. 13.47 g of a pale yellow oil were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07772262B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-6087daf0a21747a5a9e520a04e85a4ec |
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| 出典メモ | uspto-grants-2010_08 |
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