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Oxalyl chloride → 2-(4-Tert-butylphenyl)-6-nitro-3,1-benzoxazin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 2-(4-Tert-butylbenzoylamino)-5-nitrobenzoic acid | HCID 10497475 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(4-Tert-butylphenyl)-6-nitro-3,1-benzoxazin-4-one | HCID 385599 | 94% |
反応手順
To a suspension of 2-(4-tert-butylbenzoylamino)-5-nitrobenzoic acid (37.1g, 108 mmol) and N,N-dimethylformamide (0.4 mL, 5.4 mmol) in methylene chloride (200 mL) was added oxalyl chloride (10.4 mL, 119 mmol) in a dropwise manner. After stirring for 2 h, the mixture was filtered and the small amount of black solid was discarded. The filtrate was concentrated in vacuo to give 32.9 g (94%) of the title compound as a light brown solid; mp 159-61° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06313122B1 |
| 出典データセット | uspto-grants-2001_11 |
| ORD ID | ord-9846f501acf34ec9bb229ebbea2a5605 |
| 出典メモ | uspto-grants-2001_11 |