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Methyl chloroacetate → methyl 4-hydroxy-2-methyl-2H-1,2-benzothiazine-3-carboxylate 1,1-dioxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl chloroacetate | HCID 7295 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-methyl-1,2-benzisothiazol-3(2H)-one 1,1-dioxide | HCID 27290 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | methyl 4-hydroxy-2-methyl-2H-1,2-benzothiazine-3-carboxylate 1,1-dioxide | HCID 54676532 | — |
反応手順
To a solution of 2.9 g. (0.015 mole) of N-methylsaccharin and 2.63 g. (0.03 mole) of methylchloroacetate in 10 ml. of dimethylformamide at 40° C. was added over a period of two hours 864 mg. (0.036 mole) of 99% sodium hydride. Stirring was continued for two hours, maintaining a reaction temperature of 40°-50° C. The reaction mixture was quenched in 150 ml. of 5% hydrochloric acid, and the precipitated product filtered and dried, 3.41 g. (84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04376204 |
| 出典データセット | uspto-grants-1983_03 |
| ORD ID | ord-b8e61da925d74b23b717569ebd7c037e |
| 出典メモ | uspto-grants-1983_03 |