化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Carbonate → Isobutyloxycarbonyl-cyclohexylglycine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Isobutyl chloroformate | HCID 62365 | — |
| 反応物 | 2-(Cyclohexylamino)acetic acid hydrochloride | HCID 12220742 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Isobutyloxycarbonyl-cyclohexylglycine | HCID 67159202 | 94% |
反応手順
To a solution of the commercially available cyclohexylglycine hydrochloride (15 g, 77.4 mmol) in acetonitrile (320 ml) and water (320 ml) was added potassium carbonate. Isobutylchloroformate (11.1 ml, 85.1 mmol) was added to the clear solution over 15 minutes and the reaction was stirred for 17 hours. The acetonitrile was removed under reduced pressure and the remaining aqueous layer was extracted twice with ether (100 ml). The aqueous layer was then acidified to pH 1 with 6N hydrochloric acid and extracted with dichloromethane (3×300 ml). The organic layer was dried over sodium sulfate, filtered and concentrated to yield 18.64 g (94%) product as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07244721B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-4379e80e1fe9497995607e39cfd01486 |
| 出典メモ | uspto-grants-2007_07 |