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Diisopropylethylamine → (4-(6-Amino-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-5-ylamino)phenyl)(morpholino)methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-(Morpholine-4-carbonyl)aniline | HCID 577815 | — |
| 反応物 | 5-Chloro-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-6-amine | HCID 58279548 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (4-(6-Amino-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-5-ylamino)phenyl)(morpholino)methanone | HCID 58279511 | 33.9% |
反応手順
A mixture of 5-chloro-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-6-amine (1.05 g, 3.95 mmol), (4-aminophenyl)(morpholino)methanone (1.630 g, 7.90 mmol), and N,N-diisopropylethylamine (1.243 mL, 7.11 mmol) in 1,4-dioxane (60 mL) was heated at reflux for 2 days. The volatiles were removed under vacuum. To the residue was added water (60 mL). The precipitating material was collected by suction filtration. The filter cake was purified by ISCO (120 g silica gel, solid loading, 3-8% MeOH/CH2Cl2) to provide the desired product, (4-(6-amino-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-5-ylamino)phenyl)(morpholino)methanone (0.595 g, 1.339 mmol, 33.9% yield), as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08476430B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-c5739192b8854b41a2239b479b0afb0b |
| 出典メモ | uspto-grants-2013_07 |