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Diisopropylethylamine → 2-[Methyl-(2-iodo-phenyl)-amino]benzo[d][1,3]oxazin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methyl 2-isocyanatobenzoate | HCID 519494 | — |
| 反応物 | 2-iodo-N-methylaniline hydrochloride | HCID 45792406 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-[Methyl-(2-iodo-phenyl)-amino]benzo[d][1,3]oxazin-4-one | HCID 10619634 | — |
反応手順
A solution of 2-methoxycarbonylphenyl isocyanate (1.0 g, 5.6 mmol), N-methyl-2-iodoaniline, hydrochloride (1.6 g, 5.9 mmol) and N,N-diisopropylethylamine (1.1 mL, 6.3 mmol) in 100 mL of toluene was refluxed under N2 for 72 hours. The sample was concentrated, and partitioned between chloroform and 10% HCl. The chloroform was dried (MgSO4), filtered, concentrated and chromatographed (silica gel, methylene chloride) to give the title compound as a yellow solid, mp 144°-148° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05652237 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-8d09e22f28194e54908f64867acc5346 |
| 出典メモ | uspto-grants-1997_07 |