関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Dichloroaniline | HCID 11846 | — |
| 反応物 | 4,6-Dimethylpyrimidine-2-sulfonyl fluoride | HCID 14404718 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | N-(2,6-Dichlorophenyl)-4,6-dimethyl-2-pyrimidinesulfonamide | HCID 14404703 | — |
反応手順
To a solution of 2,6-dichloroaniline (1.0 g, 6.2 mmol) in dimethoxyethane (25 mL) was added butyl lithium (3.9 mL, 6.24 mmol). After 15 minutes, the solution was cooled to -30° and 4,6-dimethyl-2-pyrimidinesulfonyl fluoride (1.18 g, 6.2 mmol) was added. The mixture stirred for 12 hours with warming to 25° C. The mixture was concentrated and the residue was treated with 1N NaOH (2 mL) and extracted with ethyl acetate. The aqueous layer was acidified with 1N HCl and a solid was collected, m.p. 261°-263° C. NMR (90 MHZ) D6 -Acetone: δ 7.5 (m, 4H) and 2.5 (s, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04761173 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-061d9e615cca49ce98de4c0c3e9e94e9 |
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| 出典メモ | uspto-grants-1988_08 |
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