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Lithium Hydroxide → 6-methyl-3-(2H-1,2,3-triazol-2-yl)picolinic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | methyl 6-methyl-3-(2H-1,2,3-triazol-2-yl)-2-pyridinecarboxylate | HCID 59363722 | — |
| 溶媒 | Oxolane--water (1/1) | HCID 21881883 | — |
| 生成物 | 6-methyl-3-(2H-1,2,3-triazol-2-yl)picolinic acid | HCID 59363733 | — |
反応手順
A solution of methyl 6-methyl-3-(2H-1,2,3-triazol-2-yl)-2-pyridinecarboxylate D39 (36 mg) and LiOH (5.93 mg, 0.247 mmol) in THF/water (2:1, 3 ml) was stirred overnight. The mixture was evaporated under reduced pressure; the residue was taken up in water (2 ml) and neutralised with 1 M HCl water solution and then loaded onto a pre-conditioned C18 5 g column (the column was eluted with water and then MeOH). The methanol fractions were evaporated under reduced pressure to give the title compound D40 (34 mg) as a white solid. UPLC (Basic QC_POS—50-800): rt=0.30 minutes. peak observed: 205 (M+1). C9H8N4O2 requires 204. 1H NMR (400 MHz, MeOD) δ (ppm) 8.24 (d, 1 H), 7.99 (s, 2 H), 7.61 (d, 1 H), 2.67 (s, 3 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08133908B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-3e69663ce57c40eca2cab48ea7cc3cba |
| 出典メモ | uspto-grants-2012_03 |