関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Ethynyl-2-methylpyridine | HCID 638197 | — |
| 反応物 | 4-(Pyridin-2-yloxymethyl)phenyl-acetohydroximoyl chloride | HCID 72262870 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Methyl-5-(3-(4-(pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridine | HCID 59255526 | 46.1% |
反応手順
To a tetrahydrofuran (2 mL) solution of 5-ethynyl-2-methyl-pyridine (10 mg, 85 μmol) described in Manufacturing Example 190-1-1 were added 4-(pyridin-2-yloxymethyl)-phenyl-acetohydroximoyl chloride (31 mg, 0.11 mmol) described in Manufacturing Example 2-1-5 and triethylamine (18 μL, 0.13 mmol), which was stirred for 2 hours and 30 minutes at 50° C. Water was added to the reaction mixture at room temperature, which was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrated was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (heptane:ethyl acetate=1:1) to obtain the title compound (14 mg, 46%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07691882B2 |
|---|
| 出典データセット | uspto-grants-2010_04 |
|---|
| ORD ID | ord-51588e53f14545d4935997a03bb5c45d |
|---|
| 出典メモ | uspto-grants-2010_04 |
|---|