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3,3-Difluoropyrrolidine hydrochloride → 1-[3-Chloro-6-[2-(3,3-difluoro-pyrrolidin-1-yl)-ethoxy]-4-methoxy-2-methyl-5-(3-phenyl-propoxy)-phenyl]-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,3-Difluoropyrrolidine hydrochloride | HCID 24903482 | — |
| 反応物 | 1-[2-(2-Bromo-ethoxy)-5-chloro-4-methoxy-6-methyl-3-(3-phenyl-propoxy)-phenyl]-ethanone | HCID 59583495 | — |
| 生成物 | 1-[3-Chloro-6-[2-(3,3-difluoro-pyrrolidin-1-yl)-ethoxy]-4-methoxy-2-methyl-5-(3-phenyl-propoxy)-phenyl]-ethanone | HCID 25254374 | 16% |
反応手順
Example 34b (58 mg, 0.13 mmol) and 3,3-difluoropyrrolidine hydrochloride (2.5 eq.) were reacted as described under General Procedure J and the crude product was purified by flash chromatography (silica gel, hexane/Et2O 70:30) to afford the title compound as a pale yellow oil (10 mg, 16%). 1H NMR (300 MHz, CDCl3) δ 7.33-7.18 (m, 5H), 4.08 (t, J=6.2 Hz, 4H), 3.88 (s, 3H), 2.96 (t, J=13.4 Hz, 2H), 2.85-2.73 (m, 6H), 2.51 (s, 3H), 2.31-2.13 (m, 2H), 2.20-2.04 (m, 2H). MS (ES+) m/z 482.1 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202513B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-82aeb2a80e5244c58bef44690a802cf5 |
| 出典メモ | uspto-grants-2012_06 |