関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | 2-Methoxypyridine | HCID 74201 | — |
| 反応物 | [2-(Methoxymethyl-carbamoyl)-ethyl]-carbamic acid tert-butyl ester | HCID 86584230 | — |
| 反応物 | HCID 178418348 | HCID 178418348 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [4-(2-Methoxy-pyridin-3-yl)-4-oxo-butyl]-carbamic acid tert-butyl ester | HCID 102539314 | — |
反応手順
2-Methoxypyridine (1.9 ml) and then diisopropylamine (0.1 ml) were added to a solution of methyl lithium (10 ml of a 1.6M solution in ether) in tetrahydrofuran (20 ml) at −78° C. and the solution was stirred at 0° C. for 18hand then re-cooled to −78° C. A solution of 1,1-dimethylethyl [3-(methoxymethylamino)-3-oxopropyl]-carbamate (1.6 g) in tetrahydrofuran (5 ml) was added slowly and the resultant solution was allowed to warm to −30° C. over 3.5 h, quenched with aqueous ammonium chloride and extracted with ether (three times). The combined organic extracts were dried (sodium sulphate), evaporated and purified by chromatography on silica eluting with petrol-ether gave the sub-title compound as a colourless oil (0.572 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06743939B2 |
|---|
| 出典データセット | uspto-grants-2004_06 |
|---|
| ORD ID | ord-3e38315d28f442a38cbf626afe239183 |
|---|
| 出典メモ | uspto-grants-2004_06 |
|---|