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Potassium Hydroxide → Methyl 2-[(dimethyl-amino)thioxomethoxy]-3-methylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Dimethylthiocarbamoyl chloride | HCID 27871 | — |
| 反応物 | Benzoic acid, 2-hydroxy-3-methyl-, methyl ester | HCID 31835 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 2-[(dimethyl-amino)thioxomethoxy]-3-methylbenzoate | HCID 19814654 | 80% |
反応手順
A mixture of 12 g of KOH pellets, 150 mL of methanol and 24.9 g of methyl 2-hydroxy-3-methylbenzoate (I) was stirred at room temperature for 0.5 hours. The mixture was then cooled to 5° C. and 19 g of dimethylthiocarbamoyl chloride was added in one portion. An exotherm of 5° C. was observed. The resulting mixture was stirred for 2 hours and then added to 300 mL of ice water. After filtering, the crystalline product was washed with water and oven dried to yield 30-35 g of methyl 2-[(dimethyl-amino)thioxomethoxy]-3-methylbenzoate II, (E is O, W is S) in 80-92% yield, mp 94-96° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05157119 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-3174f41418564e6594da6e392c8d9c9a |
| 出典メモ | uspto-grants-1992_10 |