関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-(Di-tert-butylphosphino)biphenyl | HCID 2734215 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 反応物 | HCID 67971350 | HCID 67971350 | — |
| 反応物 | 3-(4-Ethoxy-2-fluoro-phenoxy)-azetidine | HCID 86689018 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 86689019 | HCID 86689019 | — |
反応手順
Under an argon atmosphere a mixture of 0.080 g (0.295 mmol) (S)-3-[1-(4-bromo-phenyl)-ethyl]-1,1-dimethyl-urea (II.1), 0.073 g (0.295 mmol) 3-(4-ethoxy-2-fluoro-phenoxy)-azetidine (IX.2), 0.117 g (97%, 1.18 mmol) NaOtBu, 0.0035 g (0.118 mmol) 2-(di-tert-butylphosphino)biphenyl, 0.027 g (0.0295 mmol) tris-(dibenzylideneaceton)-dipalladium(0) in 1.5 mL 1,4-dioxane is stirred for 3 h at 80° C. Few water and methanol is added, the mixture is filtered and concentrated in vacuo. The residue is purified by HPLC (GeminiC18, methanol/water (+0.3% NH4OH)) to yield the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08530461B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-594b3b0544c2419a86b30f01cde02216 |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|
