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2,6-Difluorobenzoyl isocyanate → N-[[[4-[2-chloro-4-(trifluoromethyl)phenoxy]-2-fluorophenyl][(4-morpholinyl)thio]amino]carbonyl]-2,6-difluorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Difluorobenzoyl isocyanate | HCID 2733369 | — |
| 反応物 | [4-[2-Chloro-4-(trifluoromethyl)phenoxy]-2-fluorophenyl][(4-morpholinyl)thio]amine | HCID 15085830 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-[[[4-[2-chloro-4-(trifluoromethyl)phenoxy]-2-fluorophenyl][(4-morpholinyl)thio]amino]carbonyl]-2,6-difluorobenzamide | HCID 15085831 | 58.2% |
反応手順
2,6-Difluorobenzoyl isocyanate (1.4 g) in a 1:1 (v/v) mixture of toluene and petroleum ether (10 ml) was added to a solution of the compound produced by Example 6 (3 g) in the same solvent (15 ml), at ambient temperature. The solution was stirred for two hours and placed in a freezer overnight (-5° to 0° C.). The solvent was removed by evaporation, and the residue was chromatographed twice on silica, firstly using dichloromethane as eluant and secondly using a 1:1 (v/v) mixture of diethyl ether and petroleum ether, to yield the title compound (2.5 g), m.p. 77°-80° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04873327 |
| 出典データセット | uspto-grants-1989_10 |
| ORD ID | ord-e9749931db0e41bd93a12b737f4bde41 |
| 出典メモ | uspto-grants-1989_10 |