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7-[4-[2-(n-Benzyl-n-methylamino)-1-chloroethylidene]piperidin-1-yl]-1-cyclopropyl-6-fluoro-8-methoxy-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid trifluoroacetic acid salt → 1-Cyclopropyl-6-fluoro-8-methoxy-7-[4-(2-methylamino-ethylidene)-piperidin-1-yl]-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid trifluoroacetic acid salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 7-[4-[2-(n-Benzyl-n-methylamino)-1-chloroethylidene]piperidin-1-yl]-1-cyclopropyl-6-fluoro-8-methoxy-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid trifluoroacetic acid salt | HCID 68689766 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Formic acid methanol | HCID 18963719 | — |
| 生成物 | 1-Cyclopropyl-6-fluoro-8-methoxy-7-[4-(2-methylamino-ethylidene)-piperidin-1-yl]-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid trifluoroacetic acid salt | HCID 68692464 | 15% |
反応手順
A solution of 161 (70 mg, 0.11 mmol) in methanol/formic acid (v/v=20/1) (14 mL) was treated with 10% Pd/C (35 mg, 7.3 mmol) under nitrogen at rt and stirred for 3 h. The resulting mixture was filtered and concentrated in vacuo. The residue was purified by HPLC (reverse phase C-18 column, 35-90% acetonitrile/water containing 0.1% trifluoroacetic acid) to afford the trifluoroacetic acid salt of 221 (8.3 mg, 15%) as a yellow solid. MS 416 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732612B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-d8d84525491b41ad84594ab336ea1579 |
| 出典メモ | uspto-grants-2010_06 |