関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroacetaldehyde | HCID 33 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (R)-2-chloro-8-cyclopentyl-7-ethyl-7,8-dihydropteridin-6-amine | HCID 59389593 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (R)-3-chloro-5-cyclopentyl-6-ethyl-5,6-dihydroimidazo[1,2-f]pteridine | HCID 59389590 | — |
反応手順
(R)-2-chloro-8-cyclopentyl-7-ethyl-7,8-dihydropteridin-6-amine (177 mg, 0.64 mmol) in MeOH (1.5 mL) treated with 50% aqueous chloroacetaldehyde (131 μL, 1.3 Eq.) and the reaction mixture heated to reflux for 6 hours. A further portion of 50% aq. chloroacetaldehyde (400 μL, 3.0 Eq.) was added, and the reaction mixture heated to 68° C. overnight. NaHCO3 (aq. sat.) and EtOAc was added, and the aqueous was further extracted with EtOAc. The combined organic extracts were dried over MgSO4, filtered and concentrated in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08524902B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-3e1e8996efa2489aa28b5ccb4882deb3 |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|
