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Methyl 3-methoxy-4-(6-nitro-2,3-di-hydrobenz-1,4-oxazin-4-ylmethyl)benzoate → Methyl 4-(6-amino-2,3-dihydrobenz-1,4-oxazin4-ylmethyl)-3-methoxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 3-methoxy-4-(6-nitro-2,3-di-hydrobenz-1,4-oxazin-4-ylmethyl)benzoate | HCID 14763125 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl 4-(6-amino-2,3-dihydrobenz-1,4-oxazin4-ylmethyl)-3-methoxybenzoate | HCID 14763126 | 98.9% |
反応手順
Palladium-on-carbon (10% w/w, 0.2 g.) was added to a solution of (G) (0.69 g.) in ethyl acetate (50 ml.) in a hydrogenation bottle and the mixture hydrogenated at a pressure of 3.17 bars of hydrogen. When the uptake of hydrogen had ceased, catalyst was removed by filtration through diatomaceous earth. The filter pad was washed with ethyl acetate and the filtrate and washings were evaporated to give methyl 4-(6-amino-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl)-3-methoxybenzoate (0.625 g., 91%) as a foam; NMR: 3.1(br s,2H, NH2), 3.3(t, 2H, OCH2CH2N), 3.85(m,6H, OCH3 +CO2CH3), 4.2(t,2H, OCH2CH2N), 4.45(s, 2H, CH2 --Ar), 6.0(m,2H), 6.55(d,1H), 7.3(d,1H), 7.55(m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05583152 |
| 出典データセット | uspto-grants-1996_12 |
| ORD ID | ord-b3b7f89df3a640948a863449c2f59a11 |
| 出典メモ | uspto-grants-1996_12 |