化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → Gsk-269984A
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 6-(5-chloro-2-((4-chloro-2-fluorobenzyl)oxy)benzyl)picolinate | HCID 59384237 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Gsk-269984A | HCID 23696973 | — |
反応手順
117 g (0.27 mol) of ethyl 6-[(5-chloro-2-{[(4-chloro-2-fluorophenyl)methyl]oxy}phenyl)-methyl]-2-pyridinecarboxylate were dissolved in ethanol (1 litre) (heating required) and 2M sodium hydroxide (200 ml) was added while still hot. Left to crystallise, and when at room temperature was diluted with an equal volume of water. After one hour at room temperature the solid was filtered off and washed with ethanol/water (1:3). MLS (mother liquors) were evaporated to remove ethanol, the solid was filtered off and the two lots were combined and washed with water and ether. Dried in a vacuum oven for 16 hours at 40° C. and 3 days at 60° C. Yield 110.5 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07759369B2 |
| 出典データセット | uspto-grants-2010_07 |
| ORD ID | ord-08e2f34df64749dcae11d5a7e9596421 |
| 出典メモ | uspto-grants-2010_07 |