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Methyl 2-nitroacetate → Methyl nitro(1,3-oxazinan-2-ylidene)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 2-nitroacetate | HCID 17206 | — |
| 反応物 | 5,6-dihydro-2-(methylthio)-4H-1,3-oxazine | HCID 21816718 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | Methyl nitro(1,3-oxazinan-2-ylidene)acetate | HCID 71444191 | — |
反応手順
A mixture of 25 g of 5,6-dihydro-2-(methylthio)-4H-1,3-oxazine (Clapp, et al., J. Heterocyclic Chemistry, 5, 107 (1968)), 25 g of methyl nitroacetate and a catalytic amount of zinc chloride was heated to 90° over one hour and maintained at that temperature for an additional hour. The mixture then was cooled and triturated with ether to effect crystallization. The solid was recrystallized from ethanol to give methyl nitro(tetrahydro-2H-1,3-oxazin-2-ylidene)acetate (1A), as a yellow solid, m.p.: 132°-3°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03976772 |
| 出典データセット | uspto-grants-1976_08 |
| ORD ID | ord-c9185385c0a245acabbfac2212c48638 |
| 出典メモ | uspto-grants-1976_08 |