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Acetic Acid → 6-Fluoro-8-{4-[1-(8-quinolinyl)-4-piperidinyl]-1-piperazinyl}quinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | 6-Fluoro-8-(piperazin-1-yl)quinoline | HCID 58975488 | — |
| 反応物 | 1-Quinolin-8-yl-piperidin-4-one | HCID 59204842 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 6-Fluoro-8-{4-[1-(8-quinolinyl)-4-piperidinyl]-1-piperazinyl}quinoline | HCID 12004112 | 45.4% |
反応手順
To a solution of 0.247 g of 6-fluoro-8-piperazino-quinoline (Step 3) in 10 mL of dichloroethane, was added 0.226 g of 1-quinolin-8-yl-piperidin-4-one (Example A, Step 6, above) followed by 0.274 g of sodium triacetoxyborohydride and 0.1 mL acetic acid. The reaction was stirred at room temperature overnight. It was quenched with 1N NaOH, and the product was extracted with CH2Cl2. The organic phase was washed with water and dried over magnesium sulfate. The product crystallized and filtered to give 0.200 g of the desired product. Mp: 211° C.; MS (ES) m/z (relative intensity): 442 (M++−H, 100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07671056B2 |
| 出典データセット | uspto-grants-2010_03 |
| ORD ID | ord-15e277b2b500461b9ea0927b56b83a7f |
| 出典メモ | uspto-grants-2010_03 |