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Lithium hydroxide, monohydrate → 4'-(Tert-butyl-methyl-sulfamoyl)-biphenyl-4-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | 4'-(tert-Butyl-methyl-sulfamoyl)-biphenyl-4-carboxylic acid methyl ester | HCID 57980165 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | 4'-(Tert-butyl-methyl-sulfamoyl)-biphenyl-4-carboxylic acid | HCID 57980106 | 88.3% |
反応手順
Procedure T′: A 15 mL dioxane/H2O (2:1) mixture of 4′-(tert-butyl-methyl-sulfamoyl)-biphenyl-4-carboxylic acid methyl ester (318 mg, 0.88 mmol) and LiOH—H2O (46 mg, 1.1 mmol) is stirred at room temperature overnight. The reaction mixture is concentrated, is diluted with EtOAc, shaken with 1 NHCl, and the layers are separated. The 1 N HCl layer is extracted with EtOAc and the combined organic layers are washed with brine, then dried over Na2SO4 and evaporated to give the intermediate 4′-(tert-butyl-methyl-sulfamoyl)-biphenyl-4-carboxylic acid (270 mg, 88% yield). MS (ES−) 346.1 (M−H)−
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07632857B2 |
| 出典データセット | uspto-grants-2009_12 |
| ORD ID | ord-b46e8f3edaf942449472ad2d7c433f44 |
| 出典メモ | uspto-grants-2009_12 |