参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 反应物 | 苄硫醇 | HCID 7509 | — |
| 反应物 | 碳酸钾 | HCID 11430 | — |
| 反应物 | 2-氯烟酸 | HCID 76258 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 产物 | 2-苄硫基烟酸 | HCID 757779 | 71.49% |
反应步骤
In a stirred suspension of 96.37 g potassium carbonate in 700 gm dimethyl formamide, 100 gm 2-chloro nicotinic acid was charged. A solution of 82.38 g benzyl mercaptan in 300 gm dimethyl formamide was added in a period of two hours maintaining reaction temperature 80-90° C. The temperature of the reaction was raised up to 140° C. and then maintained for another three hours. 500 g water was added after completion of the reaction and solvent recovery. Product precipitation achieved by lowering the pH of the reaction mass by using dilute HCl. Product 2-(Phenyl methyl thio)-3-pyridine carboxylic acid precipitated completely till pH 4.5. After filtration and washing, cake was dried to get 110 g white to off white solid product 2-(Phenyl methyl thio)-3-pyridine carboxylic acid with 71.49% yield (Assay by HPLC 99.23%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US07745631B2 |
|---|
| 来源数据集 | uspto-grants-2010_06 |
|---|
| ORD ID | ord-f8d5243b73db43b5bb6aefa2d11b2d10 |
|---|
| 来源说明 | uspto-grants-2010_06 |
|---|