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Water → 4-Methoxybenzo[d][1,3]dioxole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Bromochloromethane | HCID 6333 | — |
| 反応物 | 3-Methoxycatechol | HCID 13622 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Methoxybenzo[d][1,3]dioxole | HCID 592478 | — |
反応手順
A mixture of 3-methoxy-benzene-1,2-diol (1.161 g, 8.28 mmol) in DMF (10 mL) was added to bromo-chloro-methane (611 ul, 1.1 equivalents) and stirred at 90 degrees Celsius for 4 hours. The mixture was poured into water and extracted with dichloromethane. The organic layer was poured thru a phase separator cartridge and concentrated to dryness. The crude product is a yellow liquid. The liquid was purified by column chromatography yielding 1.21 g, (96%). 1H-NMR (DMSO, 500 MHz) 6.7 (t, 1H), 6.63 (d, 1H), 6.58 (d, 1H), 5.97 (s, 2H), 3.83 (s, 3H) HPLC (method A) 2.86 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07902239B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-8b088c76980d4f5fa34226426361b0f4 |
| 出典メモ | uspto-grants-2011_03 |