関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 反応物 | 2-(1-bromopropyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one | HCID 66864208 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-(1-bromopropyl)-3-iodo-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one | HCID 66864144 | 90.5% |
反応手順
A mixture of 2-(1-bromopropyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (3.46 g, 12.3 mmol) and N-iodosuccinimide (4.15 g, 18.4 mmol) in acetonitrile (100 mL) was stirred at 80° C., under nitrogen, overnight. After removal of acetonitrile in vacuum, the resulting solid was dissolved in methylene chloride, washed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine; and then the organic layers dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure to provide the desired product (4.53 g, 90.4%). LCMS calculated for C12H13BrIN2O (M+H)+: m/z=406.9. Found: 407.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434746B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-a1a37df2a7c047c4a48b07db83119876 |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|