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Formic Acid → HCID 178523823、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | HCID 178511725 | HCID 178511725 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178523823 | HCID 178523823 | 66.4% |
反応手順
A mixture of 6.8 ml (0.072 mol) acetic acid anhydride and 2.8 ml (0.072 mol) formic acid is heated for 2 h to 60° C. and thereafter mixed, with cooling at 5° C., with 1.9 g (0.012 mol) trans-4-nitroxycyclohexylamine. One leaves to stir overnight at room temperature, subsequently dilutes with 100 ml ethyl acetate and adds 100 ml of water thereto. After neutralisation with saturated sodium hydrogen carbonate solution, the organic phase is dried with sodium sulphate and distilled off in a vacuum. After trituration with ether, the crystals are filtered off with suction. One obtains 1.5 g of the title compound of the m p 148°-150° C., i.e. 66% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05411989 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-e1b24c9a3ef84fc4ae523d33295482bf |
| 出典メモ | uspto-grants-1995_05 |