Potassium Carbonate → Tert-butyl 4-(cyclopropylmethyl)piperazine-1-carboxylate
反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Cl[CH2:21][CH:22]1[CH2:24][CH2:23]1>ClCCl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:21][CH:22]2[CH2:24][CH2:23]2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]参加物
実験手順
1-Tertbutoxycarbonylpiperazine (6a) (1.86 g, 10 mmol) was dissolved in dichloromethane (20 mL), and anhydrous potassium carbonate (829 mg, 6 mmol) was added. The dichloromethane solution of chloromethyl cyclopropane (7a) (1.1 mL, 12 mmol) was added dropwise, and reacted overnight at room temperature, after that, the reaction mixture was washed with water. The water layer was extracted with dichloromethane for twice, the organic phases were combined, washed successively with 50 mL saturated sodium bicarbonate solution and saturated sodium chloride solution for three times, dried with anhydrous sodium sulfate. Column chromatography (petroleum ether:ethyl acetate 2:1) was performed to isolate white solid powder 1-tertbutoxycarbonyl-4-(cyclopropylmethyl)piperazine (7b), 2.01 g white solid (yield 79.0%). ESI-MS m/z calculated for: 240.18. found: 241.05 [M+H]+.
後処理
- customreacted overnight at room temperature
- washafter that, the reaction mixture was washed with water
- extractionThe water layer was extracted with dichloromethane for twice, the organic phases
- washwashed successively with 50 mL saturated sodium bicarbonate solution and saturated sodium chloride solution for three times
- dry with materialdried with anhydrous sodium sulfate
出典と根拠
- ORDレコード
- ord-a7d66c35fb7446b5992eb239529631d2
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09187430B2
反応ノート
読み込み中…