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Methanesulfonic Acid → 1-Cyclopropyl-6,8-difluoro-7-[3-(1,2,4-triazol-1-yl) pyrrolidin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 1-Cyclopropyl-6,8-difluoro-7-[3-(1,2,4-triazol-1-yl) pyrrolidin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid | HCID 19005957 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 1-Cyclopropyl-6,8-difluoro-7-[3-(1,2,4-triazol-1-yl) pyrrolidin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methanesulfonate | HCID 86748096 | — |
反応手順
1-cyclopropyl-6,8-difluoro-7-[3-(1,2,4-triazol -1-yl)pyrrolidin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (20 mg, 0.05 mmol) was dissolved in 2 ml of chloroform and to this was added 4 ml of methanesulfonic acid in chloroform. The suspension formed was stirred at room temperature for five hr. The solid was collected to yield 12 mg of white solid after drying very well in the oven, m.p. 208.5°-210° C. 1H NMR (CD3OD) δ: 9.54 (s, 1H), 8.78 (s, 1H), 8.64 (s, 1H), 7.81 (dd, 13.8, 2.3Hz, 1H), 5.47-5.3 (m, 1H), 4.5-3.8 (m, 5H), 2.88-2.5 (m, 2H), 2.7 (s, 3H), 1.4-1.1 (m, 4H). Anal. calcd. for C20H21F2N5O6S . H2O: C, 46.60; H, 4.50; N, 13.59.Found: C, 46.75; H, 4.38; N, 13.51.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05342846 |
| 出典データセット | uspto-grants-1994_08 |
| ORD ID | ord-2b08be761698415f88627290a75c638f |
| 出典メモ | uspto-grants-1994_08 |