関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | 4-Chloro-9H-dipyrido[2,3-b;4',3'-d]pyrrole-6-carboxylic acid methyl ester | HCID 58364968 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Chloro-9H-dipyrido[2,3-b;4',3'-d]pyrrole-6-carboxylic acid | HCID 58365083 | 98% |
反応手順
A mixture of 4-chloro-9H-dipyrido[2,3-b;4′,3′-d]pyrrole-6-carboxylic acid methyl ester (0.73 g, 2.8 mol) and lithium hydroxide (0.38 g, 9.0 mmol) in tetrahydrofuran (15 mL) and water (3 mL) was heated at 50° C. for 1.5 hours. The mixture was allowed to cool to ambient temperature, treated with hydrochloric acid (1M, 9 mL) and evaporated in-vacuo to afford a grey solid (0.68 g, 98%). LCMS (Method B): RT=2.98 min, M+H+=248. 1H NMR (400 MHz, DMSO-d6): 12.98 (s, 1H), 9.05 (d, J=1.0 Hz, 1H), 8.95 (d, J=1.0 Hz, 1H), 8.63 (d, J=5.3 Hz, 1H), 7.54 (d, J=5.3 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09440976B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-68314c3bc0f14cf7b38b9ab12b780a2a |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|