関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | 6-Chloro-5-methylpyridine-2-carboxylic acid | HCID 18324437 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-Methyl-6-sulfo-pyridine-2-carboxylic acid | HCID 86674744 | 111.2% |
反応手順
6-chloro-5-methyl-pyridine-2-carboxylic acid (0.85 g, 4.97 mmol) and sodium sulfite (CAN 7757-83-7, 1.5 g, 11.9 mmol) were added to water (3 mL) and ethanol (3 mL). The mixture was heated to 180° C. for 4 h in a sealed tube. After that the mixture was cooled to room temperature and a solid precipitated that was removed by filtration. The filtrate was concentrated and added to water (20 mL). The aqueous phase was washed with ethyl acetate (2×20 mL). Subsequently the aqueous phase was adjusted to pH=2 with 2 N hydrochloric acid. Water was removed in vacuo to give the product as solid (1.2 g); MS (EI): m/e=218.0 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09321727B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-61d4bf3cf5e343f7852222a883dd8bdf |
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| 出典メモ | uspto-grants-2016_04 |
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