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Hydrochloric Acid → ethyl N-(2,4,6-trimethylphenyl-acetyl)-thiomorpholine-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,4,6-Trimethylbenzeneacetyl chloride | HCID 11030754 | — |
| 反応物 | Ethyl thiomorpholine-3-carboxylate | HCID 13604869 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | ethyl N-(2,4,6-trimethylphenyl-acetyl)-thiomorpholine-3-carboxylate | HCID 19896683 | 94.7% |
反応手順
175.3 g (1 mol) of ethyl thiomorpholine-3-carboxylate are dissolved in 1000 ml of abs. THF, 140 ml (1 mol) of triethylamine are added and 198.5 g (1 mol) of mesitylene acetyl chloride are added dropwise at 0° to 10° C. The mixture is subsequently stirred at room temperature for a further 1 h and poured into 4.5 1 of ice water and 500 ml of 1 N HCl, and a flocculant, strongly water-containing product is filtered off with suction, taken up in methylene chloride, dried using MgSO4 and concentrated on a rotary evaporator. In this manner, 317.2 g (=94.7% of theory) of ethyl N-(2,4,6-trimethylphenyl-acetyl)-thiomorpholine-3-carboxylate are obtained as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05116836 |
| 出典データセット | uspto-grants-1992_05 |
| ORD ID | ord-220b73f5198c4dcfbfad3c7165d31af5 |
| 出典メモ | uspto-grants-1992_05 |