関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Tert-butyl-6-chlorobenzoxazole-7-sulfonyl chloride | HCID 23447791 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Tert-butyl-6-chlorobenzooxazole-7-sulfonic acid dimethylamide | HCID 67128555 | 93% |
反応手順
12.9 ml (93 mmol; 3.0 eq) of triethylamine and 93 ml of 2 M dimethylamine in tetrahydrofuran were added dropwise to a solution of 9.55 g (31 mmol; 1.0 eq) of 2-tert-butyl-6-chlorobenzoxazole-7-sulfonyl chloride in 200 ml of tetrahydrofuran cooled to 0° C. The reaction medium was stirred at 0° C. for 3 hours and was then treated with water. The reaction medium was extracted with ethyl acetate. The organic phases were combined, washed with water, dried over magnesium sulfate, filtered and evaporated. 9.12 g of 2-tert-butyl-6-chlorobenzooxazole-7-sulfonic acid dimethylamide were obtained in the form of a beige solid. Yield=93%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09388149B2 |
|---|
| 出典データセット | uspto-grants-2016_07 |
|---|
| ORD ID | ord-34117f0ee92d4c009f760ed6ee7a9f08 |
|---|
| 出典メモ | uspto-grants-2016_07 |
|---|