関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 6-Methoxy-4-methylpyridin-3-amine | HCID 243170 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 86717590 | HCID 86717590 | 94.6% |
反応手順
To a 100 mL flask was added 4-methyl-6-(methyloxy)-3-pyridinamine (850 mg, 6.15 mmol), pyridine (10 mL) and then ethyl chloroformate (0.650 mL, 6.77 mmol) portionwise. The reaction mixture was stirred for 1 h at 0° C. The reaction mixture was then concentrated and partitioned between ammonium chloride and DCM, and the aqueous layer was extracted with DCM (2×). The combined organics layers were washed with brine (1×), eluted through a phase separator then concentrated to afford ethyl [4-methyl-6-(methyloxy)-3-pyridinyl]carbamate (1.223 g, 90% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09187464B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-c3e18235a1ff407ebd7487b7b56283d5 |
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| 出典メモ | uspto-grants-2015_11 |
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