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N-Methylisopropylamine → 3-[4-Chloro-2-fluoro-5-{[isopropyl(methyl)amino]carbonylaminosulfonyl}phenyl]-1-methyl-2,4-dioxo-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-Methylisopropylamine | HCID 78485 | — |
| 反応物 | 2-Chloro-4-fluoro-5-[3,6-dihydro-3-methyl-2,6-dioxo-4-trifluoromethyl-(2H)-pyrimidin-1-yl]benzenesulfonylisocyanate | HCID 58709439 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 3-[4-Chloro-2-fluoro-5-{[isopropyl(methyl)amino]carbonylaminosulfonyl}phenyl]-1-methyl-2,4-dioxo-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine | HCID 58709437 | — |
反応手順
With stirring, 1.0 g (2.34 mmol) of 2-chloro-4-fluoro-5-[3,6-dihydro-3-methyl-2,6-dioxo-4-trifluoromethyl-(2H)-pyrimidin-1-yl]benzenesulfonyl isocyanate in 1,2-dichloroethane was added to a solution of 0.34 g (4.68 mmol) of N-methylisopropylamine in 1,2-dichloroethane, and the mixture was stirred overnight. The reaction mixture was concentrated, the residue was taken up in methylene chloride and 0.5N hydrochloric acid was added. The organic phase was then dried and the solvent was removed. This gave 0.5 g (42% of theory) of the title compound as a colorless solid (m.p.: 145° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741485B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-dfb6cfc1a7aa40f98611b46339d471c2 |
| 出典メモ | uspto-grants-2010_06 |