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Sulfuric Acid → 3,3,3-Trinitropropyl Pentafluorothioacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 3,3,3-Trinitropropan-1-ol | HCID 13086411 | — |
| 反応物 | Pentafluorothioacetic acid | HCID 86743239 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 3,3,3-Trinitropropyl Pentafluorothioacetate | HCID 57174425 | 95.6% |
反応手順
A mixture of 0.57 g (0.003 mole) of pentafluorothioacetic acid, 1.2 g (0.006 mole) of 3,3,3-trinitropropanol and 0.3 ml of concentrated sulfuric acid in 10 ml of 1,2-dichloroethane was stirred at reflux temperature for 24 hr in a flask with a reverse Dean Stark trap attached. The reaction mixture was cooled and the organic layer was decanted from the insoluble sulfuric acid. After the removal of volatiles from the organic layer, the residue (oil) was chromatographed on silica gel 40 using methylene chloride as eluent to give 0.99 g (89%) of product, mp 32° C.;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04849540 |
| 出典データセット | uspto-grants-1989_07 |
| ORD ID | ord-abdf7bfce7b04fe9a4f601d7cb38d772 |
| 出典メモ | uspto-grants-1989_07 |