関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chloro-6-methylpyridine-4-carboxylic acid | HCID 141209 | — |
| 反応物 | 1,1-bis(1,1-dimethylethoxy)-N,N,N-trimethylamine | HCID 547712 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Chloro-6-methyl-isonicotinic acid tert-butyl ester | HCID 86040366 | — |
反応手順
N,N-dimethylformamide-di-tert.-butyl-acetal (19 mL, 80 mmol) is added during 40 min to a hot (65° C., flask temperature) suspension of 2-chloro-6-methyl-isonicotinic acid (3.40 g, 19.8 mmol) in dry toluene (100 mL). The clear orange solution is stirred at 80° C. for 48 h, cooled to rt and diluted with toluene (100 mL). The solution is washed with water (2×40 mL), sat. aq. NaHCO3 (3×30 mL) and sat. aq. NaCl (25 mL), dried (Na2SO4), filtered and evaporated. The residue is purified by FC (SiO2, DCM-MeOH) to give 2-chloro-6-methyl-isonicotinic acid tert-butyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08178562B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-ddf186e5a9d84329b922b4a73876dabe |
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| 出典メモ | uspto-grants-2012_05 |
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