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Iodine → Tert-butyl 3-(3-chloro-4-fluorophenyl)-3-hydroxypyrrolidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Tert-butyl 3-oxopyrrolidine-1-carboxylate | HCID 471360 | — |
| 反応物 | 4-Bromo-2-chloro-1-fluorobenzene | HCID 3543065 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Tert-butyl 3-(3-chloro-4-fluorophenyl)-3-hydroxypyrrolidine-1-carboxylate | HCID 67402987 | 41.1% |
反応手順
Preparation according to Preparation 1. 1-Bromo-3-chloro-4-fluorobenzene (5 g, 23.9 mmol) in dry tetrahydrofuran (100 ml), magnesium turnings (0.57 g, 23.9 mmol) and one crystal of iodine. 1-N-boc-3-pyrrolidone (4.41 g, 23.9 mmol) in dry tetrahydrofuran (50 ml). The crude product was purified by flash column chromatography on silica gel (ethyl acetate/isooctane, 1:9 to 1:1) gave the title compound (3.1 g, 41%). MS m/z (rel. intensity, 70 eV) 214 (16), 157 (21), 143 (19), 129 (11), 57 (bp).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09035073B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-cfdbfb2a6ba14e6280491e052a703aa9 |
| 出典メモ | uspto-grants-2015_05 |