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Methanol → 2-Amino-5-chloro-3-methoxypyrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 3-Bromo-5-chloropyrazin-2-amine | HCID 10488609 | — |
| 生成物 | 2-Amino-5-chloro-3-methoxypyrazine | HCID 10797036 | — |
反応手順
Sodium (2.82 g) was dissolved in dry methanol (50 ml) under argon and 2-amino-3-bromo-5-chloropyrazine (1.68 g) was added in small portions with stirring. The stirred solution was heated at reflux under an atmosphere of argon for 4 hours. The solution was allowed to cool to ambient temperature and water (10 ml) was added. Volatile material was removed by evaporation and water (10 ml) was added to the residue. The mixture was extracted with dichloromethane (3×50 ml) and the combined extracts were dried (MgSO4) and evaporated to give 2-amino-5-chloro-3-methoxypyrazine (1.28 g), m.p. 102-103° C.; 1H NMR (d6 -DMSO): 3.90 (s, 3H), 7.53 (s, 1H); mass spectrum (+ve CI): 160 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06060475 |
| 出典データセット | uspto-grants-2000_05 |
| ORD ID | ord-08e1b076b4574af89cff437f058b09bf |
| 出典メモ | uspto-grants-2000_05 |