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乙醛酸 → 2-羟基-6-氯喹喔啉
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 乙醛酸 | HCID 760 | — |
| 反应物 | 4-氯-1,2-苯二胺 | HCID 7263 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | 2-羟基-6-氯喹喔啉 | HCID 75507 | — |
反应步骤
Following the procedure of J. Med. Chem., 24, 93 (1981), glyoxylic acid (29.4 ml) is added to a solution of 4-chloro-1,2-phenylenediamine (38.0 g) and methanol (1.87 L) at 15°. The solution is stirred for 24 hr at 20°-25° and is concentrated. The residue is washed with water (4×608 ml), isopropanol (145 ml), and dried under reduced pressure to give a solid. Two successive recrystallizations from hot (ca 90°) 2-methoxyethanol (1.49 l and 0.927 l) gives the title compound, NMR (DMSO-d6) 12.55, 8.22, 7.86, 7.62 and 7.32 δ.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05541324 |
| 来源数据集 | uspto-grants-1996_07 |
| ORD ID | ord-dfe57345803249f98b2cd614b0273258 |
| 来源说明 | uspto-grants-1996_07 |