関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | HCID 178470035 | HCID 178470035 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | HCID 178516647 | HCID 178516647 | 99.5% |
反応手順
2,4-Dihydroxy-6-trifluoromethyl-nicotinic acid ethyl ester (62 g/247 mmols) was added in several portions over 30 mins to 6M HCl(aq) (620 mls) at reflux. The resulting mixture was then heated at 100° C. overnight with vigorous stirring to obtain complete solution. The solution was then allowed to cool and concentrated in vacuo to a white solid. This was slurried in water (250 mls) and adjusted to pH 7 with conc. ammonia to get heavy white suspension. The resulting solid was collected by filtration, rinsed through with fresh water, and dried to provide the title compound (44.0 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07691877B2 |
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| 出典データセット | uspto-grants-2010_04 |
|---|
| ORD ID | ord-f3aba04b1d624006845308eb4c12e6ca |
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| 出典メモ | uspto-grants-2010_04 |
|---|