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Phosgene → 1-chloro-N-(2-chloro-4-fluoro-5-isocyanatophenyl)methanesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | N-(5-amino-2-chloro4-fluorophenyl)-1-chloromethanesulfonamide | HCID 11000212 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-chloro-N-(2-chloro-4-fluoro-5-isocyanatophenyl)methanesulfonamide | HCID 11077402 | 95.5% |
反応手順
To a stirred solution of phosgene (68 mmol) in 35 mL toluene was added the title compound of Step D (4.2 g, 15.4 mmol) in 80 mL toluene at 0° C. and the reaction was stirred at room temperature overnight. The temperature was then raised to 70° C. for 4 h. After cooling to room temperature, the reaction mixture was filtrated and the solvent was removed under reduced pressure. Drying of the white precipitate under reduced pressure yielded the title compound of Step E (4.4 g, 95%) melting at 101.5-102.5° C. 1H NMR (CDCl3) δ 7.5 (d, 1H), 7.3 (d, 1H), 7.0-6.9 (br s, 1H), 4.64.5 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06060432 |
| 出典データセット | uspto-grants-2000_05 |
| ORD ID | ord-876da175843b498091fe36facd3e0ee5 |
| 出典メモ | uspto-grants-2000_05 |