関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 6-Bromo-1-phenoxyisoquinoline | HCID 22665862 | — |
| 生成物 | 1-Amino-6-bromoisoquinoline | HCID 22607616 | 71.8% |
反応手順
A mixture of 12 g of 1c and 27 g of ammonium acetate was heated at 150° C. for 14 hours. After cooling to room temperature aqueous 3N NaOH was added and the mixture was extracted with ethyl acetate. The ethyl acetate extract was washed with brine and aqueous 2N hydrochloric acid was added until pH2-3. The acid aqueous layer was separated, made basic (pH 10) with aqueous 2N NaOH and extracted with ethyl acetate. The ethyl acetate layer was washed with brine, dried (MgSO4) and concentrated to give 6.4 g of 1d. 1H-NMR 200 MHz (CDCl3) δ: 5.1 (2H, br s), 6.96 (1H, dd, J=6 Hz and J=]Hz), 7.54-7.70 (2H, m), 7.88 (1H, d, J=2 Hz), 7.98 (1H, d, J=6 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06194409B1 |
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| 出典データセット | uspto-grants-2001_02 |
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| ORD ID | ord-25fe104964ac4f3e8ad5a7850535d88c |
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| 出典メモ | uspto-grants-2001_02 |
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