関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-methylthiophen-3-amine | HCID 642344 | — |
| 反応物 | 2-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenyl | HCID 2734217 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 反応物 | HCID 86670921 | HCID 86670921 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 68226672 | HCID 68226672 | — |
反応手順
A mixture of {4-[3-(6-bromo-pyridin-2-yl)-imidazo[1,2-a]pyrazin-8-ylamino]-cyclohexyl}-carbamic acid tert-butyl ester (from Example 40 supra) (0.244 g, 0.5 mmol), compound thiophen-3-yl-methylamine (0.113 g, 1.0 mmol), Pd2(dba)3 (30 mg), Davephos (40 mg), NaOtBu (100 mg, 0.1 mmol) in dioxane (12 mL) in a sealed tube was bubbled with N2 for several minutes and then heated under N2 at 110° C. for 16 hours. The solution was then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure. The residue was purified by chromatography (CH2Cl2:MeOH, 100:1) to give [4-(3-{6-[(thiophen-3-ylmethyl)-amino]-pyridin-2-yl}-imidazo[1,2-a]pyrazin-8-ylamino)-cyclohexyl]-carbamic acid tert-butyl ester. (Yield 70 mg, 27%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08673905B2 |
|---|
| 出典データセット | uspto-grants-2014_03 |
|---|
| ORD ID | ord-3b9205c5487847f39e70bb464ea00fc6 |
|---|
| 出典メモ | uspto-grants-2014_03 |
|---|
