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Hydrochloric Acid → 3-[1-({6-Amino-3,5-dicyano-4-[4-(2-methoxyethoxy)phenyl]pyridin-2-yl}sulfanyl)ethyl]-benzenecarboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Methyl 3-[1-({6-amino-3,5-dicyano-4-[4-(2-methoxyethoxy)phenyl]pyridin-2-yl}sulfanyl)ethyl]-benzenecarboxylate | HCID 68614914 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-[1-({6-Amino-3,5-dicyano-4-[4-(2-methoxyethoxy)phenyl]pyridin-2-yl}sulfanyl)ethyl]-benzenecarboxylic acid | HCID 68047387 | — |
反応手順
150 mg (0.307 mmol) of methyl 3-[1-({6-amino-3,5-dicyano-4-[4-(2-methoxyethoxy)phenyl]-pyridin-2-yl}sulfanyl)ethyl]benzenecarboxylate (Example 65A) were dissolved in 7 ml of tetrahydrofuran. After addition of 14.7 mg (0.61 mmol) of lithium hydroxide, the mixture was stirred at RT overnight. The mixture was then stirred at 40° C. for 4 h. Using 1N hydrochloric acid, the pH of the reaction solution was adjusted to pH 4, and the clear solution was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09187428B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-9be33fa4998242058e736580ee7a34c5 |
| 出典メモ | uspto-grants-2015_11 |