Dichloromethane → HCID 59363373、化合物
反応式
[C:1]([O:5]C(=O)NC1CCCN(CC(F)(F)F)C1)(C)(C)C.CC[N:22]([CH:26]([CH3:28])C)[CH:23]([CH3:25])C.[C:29](Cl)(=[O:31])[CH3:30].[CH2:33](Cl)Cl>>[C:29]([N:22]1[CH2:23][CH2:25][C:1](=[O:5])[CH:28]([CH3:33])[CH2:26]1)(=[O:31])[CH3:30]参加物
5
反応条件
- 温度
- 25 °C
実験手順
To a suspension of the product of step 1 in DCM at 0° C., DIPEA (4 eqv) was added slowly and stirred for 30 minutes at 25° C. The reaction mixture was cooled again to 0° C. and acetyl chloride (1.1 eqv) was added slowly. The resulting mixture was stirred at 25° C. for 16 hrs before being quenched by addition of saturated aqueous NaHCO3. The aqueous layer was back extracted three times with DCM. The combined organics were washed with H2O, dried (Na2SO4), filtered and evaporated. The residue was purified by SiO2 flash chromatography to give racemic 1-acetyl-3-methyl-piperidin-4-one (94% over two steps).
後処理
- temperatureThe reaction mixture was cooled again to 0° C.
- stirringThe resulting mixture was stirred at 25° C. for 16 hrs
- custombefore being quenched by addition of saturated aqueous NaHCO3
- extractionThe aqueous layer was back extracted three times with DCM
- washThe combined organics were washed with H2O
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customevaporated
- customThe residue was purified by SiO2 flash chromatography
出典と根拠
- ORDレコード
- ord-fcecddb673734e6fbecb6ae7b1435cca
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08012974B2
反応ノート
読み込み中…