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Cyanogen Bromide → 7-methoxy-1H-1,3-benzodiazol-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyanogen Bromide | HCID 10476 | — |
| 反応物 | 6-Nitro-o-anisidine | HCID 85491 | — |
| 反応物 | 3-Methoxybenzene-1,2-diamine | HCID 184268 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | 7-methoxy-1H-1,3-benzodiazol-2-amine | HCID 52987703 | — |
反応手順
The material was prepared by the catalytic reduction of 2-methoxy-6-nitroaniline to 3-methoxybenzene-1,2-diamine using a hydrogen atmosphere at 40 psi and 10% palladium on carbon (50% w/w water) in methanol. The resulting crude diamine was subsequently reacted with cyanogen bromide in an acetonitrile-water mixture according to previous procedure and used without further purification. 1H-NMR (400 MHz, CDCl3), δ 12.40 (bs, 1H), 7.26 (d, 1H), 7.15 (t, 1H), 6.77 (d, 1H), 6.59 (bs, 2H), 3.73 (s, 3H). MS (EI): 164 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08088767B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-e7008136b1ab4a94a8523de7795829e4 |
| 出典メモ | uspto-grants-2012_01 |