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Methanol → 1-Benzothiazol-6-yl-3-(2-chloro-1,1-dimethyl-ethyl)-urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 6-Aminobenzothiazole | HCID 68288 | — |
| 反応物 | 1-Chloro-2-isocyanato-2-methyl-propane | HCID 11040747 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 1-Benzothiazol-6-yl-3-(2-chloro-1,1-dimethyl-ethyl)-urea | HCID 68789853 | 18.5% |
反応手順
Benzothiazol-6-ylamine (1.8 g, 12.00 mmol) was added portion wise to solution of 1-chloro-2-isocyanato-2-methyl-propane (2 g, 13.60 mmol) in toluene (20 mL) over a period of 5 minutes. The resulting mixture was stirred at room temperature for 2½ days. The reaction was monitored by TLC (5% MeOH in CHCl3). The reaction mixture was concentrated and extracted with ethylacetate. The organic layer was dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (1% MeOH in CHCl3) afforded 630 mg of the product (16.57% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | USRE045173E1 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-7d4430f7215241d5bbc8a1235cd54f54 |
| 出典メモ | uspto-grants-2014_09 |