関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 反応物 | 3-Hydroxy-5-chloropyridine | HCID 582305 | — |
| 反応物 | HCID 86621496 | HCID 86621496 | — |
| 生成物 | HCID 86621495 | HCID 86621495 | 36.9% |
反応手順
To a solution of 1-tert-butyl 3-methyl(2S,3S,5R)-2-[4-(4-cyano-3,5-dimethylphenyl)-3,6-dihydropyridin-1(2H)-yl]carbonyl-5-hydroxypiperidine-1,3-dicarboxylate (100 mg, 0.0002 mol) in tetrahydrofuran (0.912 mL, 0.0112 mol) was added 5-chloropyridin-3-ol (35.0 mg, 0.000270 mol), triphenylphosphine (70.8 mg, 0.000270 mol), followed by diisopropyl azodicarboxylate (0.0532 mL, 0.000270 mol). The mixture was heated at 70 Celsius overnight. After concentrated to dry, the mixture was purified on silica gel, elution with 0 to 40% EtOAc in hexane, to yield the desired product (45 mg, 32.84%). MS (ESI) (M+H) 609.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09440958B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-4c4af428e94848f48b61608bf4d97099 |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|
