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2-Thiophenecarboxylic acid, 3-(isocyanatosulfonyl)-, methyl ester → HCID 20261265、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Thiophenecarboxylic acid, 3-(isocyanatosulfonyl)-, methyl ester | HCID 157296 | — |
| 反応物 | 4-(Difluoromethoxy)-6-methylpyrimidin-2-amine | HCID 2817390 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 20261265 | HCID 20261265 | 50% |
反応手順
A solution of 6.2 g of 2-methoxycarbonyl-3-thienylsulfonylisocyanate in 50 ml of absolute tetrahydrofuran is stirred dropwise into a solution of 4.4 g of 2-amino-4-difluoromethoxy-6-methylpyrimidine in 80 ml of absolute tetrahydrofuran. During the course of this addition, the temperature of the reaction mixture rises from 20° to 26° C. After it has been stirred for another hour, the raction mixture is filtered and the filtrate is concentrated. The residue is crystallised from ethyl acetate, affording 5.3 g (50%) of N-(2-methoxycarbonyl-3-thienylsulfonyl)-N'-(4-difluoromethoxy-6-methylpyrimidin-2-yl)urea (compound 2.1) with a melting point of 178°-179° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04549898 |
| 出典データセット | uspto-grants-1985_10 |
| ORD ID | ord-3086ea1c378a4a7e855846d0a83f48ec |
| 出典メモ | uspto-grants-1985_10 |