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Sarcosine methyl ester → Methyl 6-((2-methoxy-2-oxoethyl)(methyl)amino)-5-nitronicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sarcosine methyl ester | HCID 83545 | — |
| 反応物 | Methyl 6-chloro-5-nitronicotinate | HCID 346961 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 6-((2-methoxy-2-oxoethyl)(methyl)amino)-5-nitronicotinate | HCID 58324470 | 99.5% |
反応手順
Methyl 6-chloro-5-nitronicotinate (2.0 g, 9.23 mmol) was added to methyl 2-(methylamino)acetate (1.9 g, 18.47 mmol) neat while stirring at room temperature. The viscous yellow reaction was heated to 90° C. for one hour and then allowed to cool back to room temperature. The reaction was diluted with dichloromethane (20 mL) and purified using flash column chromatography (220 g SiO2, 20-30% gradient, ethyl acetate in hexanes) to yield 2.60 g (99% yield) of the title compound as a yellow oil. [M+H] calc'd for C11H13N3O6, 284; found, 284.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822470B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-c0499d0168ab4fbd9bfe9ee366c17ebb |
| 出典メモ | uspto-grants-2014_09 |