化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 56661559、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | 4-{3-[2-(1-Methyl-5-trifluoromethyl-1H-indazol-3-ylamino)-acetylamino]-azetidin-1-yl}-cyclohexane carboxylic acid ethyl ester | HCID 56671925 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 56661559 | HCID 56661559 | — |
反応手順
4-{3-[2-(1-Methyl-5-trifluoromethyl-1H-indazol-3-ylamino)-acetylamino]-azetidin-1-yl}-cyclohexane carboxylic acid ethyl ester (from Example 32, 350 mg, 0.773 mmol) in THF (2 mL), MeOH (2 mL) and distilled water (2 mL) was treated with lithium hydroxide monohydrate (87 mg, 1.93 mmol) at room temperature for 1 hour. The reaction mixture was acidified to pH=5 and extracted with DCM:IPA (3:1) solvent three times. The combined organic layer was washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give the title compound as colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08436023B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-40a90e80670f490083cd8ad9a758354e |
| 出典メモ | uspto-grants-2013_05 |