関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1-tert-Butyl-4-Trifluoromethanesulfonlyoxy-1,2,3,6-tetrahydropyridine | HCID 18694292 | — |
| 反応物 | HCID 178431682 | HCID 178431682 | — |
| 触媒 | (1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium | HCID 6505921 | — |
| 触媒 | HCID 178454872 | HCID 178454872 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | HCID 178431684 | HCID 178431684 | 67.8% |
反応手順
To a solution of [(S)-3-(tert-butyldimethylsilanyloxy)-1-(2-fluorophenyl)propyl]-{6,6-dimethyl-4,4-dioxo-5-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)phenyl]-5,6-dihydro-4H-4lambda*6*-[1,4,3]oxathiazin-2-yl}amine (300 mg), trifluoromethanesulfonic acid 1-tert-butyl-1,2,3,6-tetrahydropyridin-4-yl ester (208 mg) and cesium carbonate (519 mg) in 3:1 dioxane/water (4 ml) were added Pd(dba)2 (31 mg) and CTC-Q-Phos (75 mg), and the mixture was stirred at 62° C. for 40 min. After dilution with ethyl acetate, the mixture was washed with water, dried using a kieselguhr cartridge and concentrated. This was followed by purification by column chromatography (ethyl acetate/heptane). This gave the product (207 mg) with a molecular weight of 658.0 g/mol (C35H52FN3O4SSi).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08895547B2 |
|---|
| 出典データセット | uspto-grants-2014_11 |
|---|
| ORD ID | ord-06d5ff6be70a409ebd1cd6a503bee4d9 |
|---|
| 出典メモ | uspto-grants-2014_11 |
|---|
