化工社化工社 化学情報印刷レポート · 研究参考用
Delta-Valerolactone → 8-chloro-2-methyl-2,3,4,4a-tetrahydro-10H-1,2-oxazino(3,2-b)(1,3)benzoxazin-10-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Delta-Valerolactone | HCID 10953 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Benzamide, 5-chloro-N,2-dihydroxy- | HCID 169935 | — |
| 反応物 | 4-Chloropentanoyl chloride | HCID 12603962 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | 8-chloro-2-methyl-2,3,4,4a-tetrahydro-10H-1,2-oxazino(3,2-b)(1,3)benzoxazin-10-one | HCID 12365950 | — |
反応手順
A mixture of 30 g. of γ -valerolactone, 30 ml. of distilled thionyl chloride and 0.5 g. of zinc chloride was heated on a steam bath overnight and then distilled at 15 mm. The distillate was redistilled at 69- 70° and 15 mm. giving 34 g. of 4-chlorovaleryl chloride. The acid chloride was reduced catalytically, reacted with 5-chlorosalicylhydroxamic acid and the resulting intermediate was ring-closed according to the method described in Example 3. The product after recrystallization from trichloroethylene weighed 8.5 g. and melted at 210- 213° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04024139 |
| 出典データセット | uspto-grants-1977_05 |
| ORD ID | ord-c9f79d7b0bf3447899fe351abbbcff38 |
| 出典メモ | uspto-grants-1977_05 |