関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | tert-Butyl 4-(2-oxo-2,3-dihydro-1H-indol-1-yl)piperidine-1-carboxylate | HCID 67472855 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Tetrahydrofuran-3-yl-3,8-diazabicyclo[3.2.1]octane | HCID 90414014 | 99% |
反応手順
Tert-butyl 4-(2-oxoindolin-1-yl)piperidine-1-carboxylate (100 mg, 0.32 mmol) in ACN is cooled down to −10° C., N-bromosuccinimide (56.47 mg, 0.32 mmol) is added and stirred at −10° C. for 2 h. The reaction mixture is diluted with dichlormethane and water. The organic layer is separated, dried and concentrated. The crude product is used for the next step without further purification. Yield 99%, m/z 395 [M+H]+, rt 1.126 min, LC-MS Method Z020_S01.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08987249B2 |
|---|
| 出典データセット | uspto-grants-2015_03 |
|---|
| ORD ID | ord-da02d577f2cd441789b6783cfa870619 |
|---|
| 出典メモ | uspto-grants-2015_03 |
|---|
