化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → 3,8-Diaza-bicyclo[3.2.1]octane-3-carboxylic acid amide hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trimethylsilyl isocyanate | HCID 70696 | — |
| 反応物 | 8-Boc-3,8-diaza-bicyclo(3.2.1)octane | HCID 15740908 | — |
| 生成物 | 3,8-Diaza-bicyclo[3.2.1]octane-3-carboxylic acid amide hydrochloride | HCID 67206024 | 99% |
反応手順
A solution of 3,8-diaza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (2.5 g, 11.7 mmol) in CH2Cl2 (50 mL) was treated with trimethylsilyl isocyanate (14 mL, 117 mmol). The resultant mixture was stirred at rt for 4 h., concentrated and redissolved in CH2Cl2 (50 mL). To this solution was added HCl (4.0 N in 1,4-dioxane, 12 mL), and the resultant mixture was stirred at rt for 3 h. Concentration afforded the title compound as a white powder (2.4 g, 99%). MS (ESI): mass calcd. for C7H13N3O, 155.1; m/z found, 156.2 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367719B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-50ff139614284bd6b080f060091df286 |
| 出典メモ | uspto-grants-2013_02 |