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Triethylamine → Thiomorpholine, N-BOC protected
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Thiomorpholine | HCID 67164 | — |
| 反応物 | tert-Butoxycarbonyl dicarbonate | HCID 86600350 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Thiomorpholine, N-BOC protected | HCID 21949316 | 87.9% |
反応手順
Thiomorpholine (5.0 ml, 53 mol) was dissolved in tetrahydrofuran (200 ml); triethylamine (8.1 ml, 58 ml) was added thereto; and the reaction mixture was stirred at room temperature. tert-Butoxycarbonyl dicarbonate (13.3 ml, 58 mmol) was added thereto and the reaction mixture was stirred at room temperature for 10 hours. The reaction mixture was concentrated under reduced pressure; and the residue was purified by silica gel column (eluent; hexane:ethyl acetate=from 80:20, 75:25 to 70:30) to yield the title compound as colorless crystals (10.4 g, 51 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07109219B2 |
| 出典データセット | uspto-grants-2006_09 |
| ORD ID | ord-1f78b47ce5144d6ba73f778e4299dc27 |
| 出典メモ | uspto-grants-2006_09 |