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Water → Methyl 3-[1-({6-amino-3,5-dicyano-4-[4-(2-methoxyethoxy)phenyl]pyridin-2-yl}sulfanyl)ethyl]-benzenecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | HCID 20428675 | HCID 20428675 | — |
| 反応物 | HCID 178496105 | HCID 178496105 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 3-[1-({6-amino-3,5-dicyano-4-[4-(2-methoxyethoxy)phenyl]pyridin-2-yl}sulfanyl)ethyl]-benzenecarboxylate | HCID 68614914 | — |
反応手順
300 mg (0.919 mmol) of 2-amino-4-[4-(2-methoxyethoxy)phenyl]-6-sulfanylpyridine-3,5-dicarbonitrile (Example 15A), 245 mg (1.01 mmol) of methyl 3-(1-bromoethyl)benzenecarboxylate (Example 61A) and 231 mg (2.76 mmol) of sodium bicarbonate were dissolved in 3 ml of DMF and the mixture was stirred at RT overnight. Water was added to the reaction mixture until a clear solution had formed. The 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-db85723dec71408d9e68fd31250524fd |
| 出典メモ | uspto-grants-2015_11 |