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Methanol → 1-Adamantyl carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Adamantanol | HCID 64152 | — |
| 反応物 | Trichloroacetyl isocyanate | HCID 76400 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Adamantyl carbamate | HCID 12437646 | 74% |
反応手順
1-Adamantanol (1.52 g, 10.0 mmol) in dichloromethane (30 mL) was mixed with trichloroacetyl isocyanate (1.40 mL, 11.8 mmol) at 0° C., then warmed to room temperature and stirred for 2 hours. After completion of the reaction, the reaction solution was evaporated under reduced pressure, and the resulting crude reaction product was mixed with methanol (15 mL) and saturated aqueous potassium carbonate and stirred at 50° C. for 1 day. After completion of the reaction, the methanol was removed by vacuum distillation, and the residue was filtered. The resulting solid was washed with water and dried under reduced pressure to give the desired product (74% yield, 2 steps).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08440666B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-4d49707e34924196974f4073021abddf |
| 出典メモ | uspto-grants-2013_05 |