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Phosphorus pentachloride → 4-chloro-2,2-dimethyl-3H-1,3-benzoxazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 2,2-dimethyl-3,4-dihydro-2H-1,3-benzoxazin-4-one | HCID 717428 | — |
| 溶媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | 4-chloro-2,2-dimethyl-3H-1,3-benzoxazine | HCID 22244720 | — |
反応手順
A solution of 2,2-dimethyl-4-keto-1,3-benzoxazine (1.77 g, 10.0 mmol) and PCl5 (2.09 g, 10.0 mmol) in POCl3 (3.0 mL) was stirred at RT for 1 h then at 50-60° C. for 2 h. The reaction was concentrated and the product distilled (90-95° C./2-3 mm Hg) to afford 4-chloro-2,2-dimethyl-3H-1,3-benzoxazine. (0.496 g, 25%) as a clear oil: 1H NMR (CDCl3, 300 MHz, ppm) 7.58 (d, 1H), 7.48 (m, 1H), 6.97 (m, 1H), 6.94 (d, 1H), 1.63 (s, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06306840B1 |
| 出典データセット | uspto-grants-2001_10 |
| ORD ID | ord-ead02719994342e38f90758e4574baa7 |
| 出典メモ | uspto-grants-2001_10 |