化工社化工社 化学情報印刷レポート · 研究参考用
Diphosgene → 2H-3,1-Benzoxazine-2,4(1H)-dione, 6-nitro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diphosgene | HCID 10426 | — |
| 反応物 | 2-Amino-5-nitrobenzoic acid | HCID 12032 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2H-3,1-Benzoxazine-2,4(1H)-dione, 6-nitro- | HCID 20821 | — |
反応手順
To the mixture of 37 g of 2-amino-5-nitrobenzoic acid in 500 mL of dioxane, under stirring 24.5 mL of diphosgene was added dropwise. The mixture was heated under reflux conditions for 6 hours then it was evaporated to dryness. The residue was suspended in 100 mL of diethyl ether and filtered off to give 41.4 g of the title product as HCl salt, m.p.: 256-259° C. LC-MS: MH+ 209; Ret. time: 5 minutes.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08071601B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-057aa17fda5d414494afbf4e55888408 |
| 出典メモ | uspto-grants-2011_12 |