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Toluene → 4-chloro-N-methylbenzothiazolone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Chlorobenzothiazolone | HCID 53400688 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-chloro-N-methylbenzothiazolone | HCID 69645010 | 98.2% |
反応手順
4-Chlorobenzothiazolone (9.28 g, 0.05 mole) was dissolved in a solution of sodium hydroxide (3.19 g, 0.075 mole) in water (220 ml), and tetra-n-butylammonium bromide (0.48 g, 0.0015 mole) and toluene (80 ml) were added thereto. Dimethyl sulfate (9.40 g, 0.075 mole) was added dropwise thereto at room temperature, and the mixture was stirred at room temperature for 1 hour, followed by phase-separation. The toluene layer was washed once with water, and the solvent was removed under reduced pressure to obtain 9.80 g of 4-chloro-N-methylbenzothiazolone as pale yellow crystals. Yield 98.2%, purity 98.2%, m.p. 130°-132° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04293702 |
| 出典データセット | uspto-grants-1981_10 |
| ORD ID | ord-a244a87ea35445fa86cd33d441bf9140 |
| 出典メモ | uspto-grants-1981_10 |