関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Bromomethylcyclopropane | HCID 81503 | — |
| 反応物 | 2-Iodo-6-methylsulfonylpyridin-3-ol | HCID 118022372 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(Cyclopropylmethoxy)-2-iodo-6-methylsulfonylpyridine | HCID 118022516 | 84.8% |
反応手順
A mixture of 2-iodo-6-methylsulfonylpyridin-3-ol (500.0 mg, 1.67 mmol), bromomethylcyclopropane (248.4 mg, 1.84 mmol) and K2CO3 (461.3 mg, 33.4 mmol) in ACN (15 mL) was stirred at 80° C. for 4 hrs. Water (30 mL) was added and the mixture was extracted with EtOAc (30 mL×3). The combined organic layers were washed with brine (30 mL), dried over Na2SO4, filtered and concentrated to give the title compound (500.0 mg, 84.8%). 1H NMR (CDCl3, 400 MHz) δ 7.96 (d, J=8.8 Hz, 1H), 7.52 (d, J=8.4 Hz, 1H), 4.09 (d, J=6.8 Hz, 2H), 3.22 (s, 3H), 1.36-1.22 (m, 1H), 0.69-0.57 (m, 2H), 0.43-0.37 (m, 2H). LCMS: 354.0 (M+1)+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09115114B2 |
|---|
| 出典データセット | uspto-grants-2015_08 |
|---|
| ORD ID | ord-cbaca222dea84f609941eca25eeba7e9 |
|---|
| 出典メモ | uspto-grants-2015_08 |
|---|