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Methanol → 2-(Methoxymethyl)-4-nitrophenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 2-(Chloromethyl)-4-nitrophenol | HCID 76305 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Methoxymethyl)-4-nitrophenol | HCID 11355878 | — |
反応手順
18.7 g (0.1 mol) of 2-chloromethyl-4-nitrophenol and 50 ml of pure methanol were mixed together and refluxed for 2 hours 30 minutes. 37 ml of sodium methoxide (0.2 mol, 5.4 N solution in MeOH) were added and the mixture was refluxed for another 30 minutes. The resulting mixture was cooled in an ice bath and diluted with 350 ml of water, and the insoluble matter formed was filtered off. The filtrate was acidified with acetic acid (10 ml). The crystalline product was filtered off by suction, reslurried in ice-cold water and then dried over P2O5 at 40° C. 11.4 g of crude products were isolated and then recrystallized from 15 ml of isopropyl acetate to give 7.5 g of expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07445645B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-0a0551b5bf3049c0a58006b54583054c |
| 出典メモ | uspto-grants-2008_11 |