反応 #89755

反応方程式

(2S,3S,5S)-5-tert-butoxy-3-(methoxycarbonyl)piperidine-2-carboxylic acid

1-phenyl-piperazine

benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate

N,N-dimethylformamide

N,N-diisopropylethylamine

→

methyl(2S,3S,5S)-5-tert-butoxy-2-[(4-phenylpiperazin-1-yl)carbonyl]piperidine-3-carboxylate

反応条件

後処理

1. 1
   その他quenched with water
2. 2
   抽出The mixture was extracted with ethyl acetate
3. 3
   洗浄The combined organic layers were washed with brine
4. 4
   その他dried
5. 5
   濃縮concentrated
6. 6
   その他to dry

実験手順

To a mixture of (2S,3S,5S)-5-tert-butoxy-3-(methoxycarbonyl)piperidine-2-carboxylic acid (43.0 mg, 0.000166 mol), 1-phenyl-piperazine (0.03166 mL, 0.0002073 mol) and benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (0.09168 g, 0.0002073 mol) in N,N-dimethylformamide (0.40 mL, 0.0052 mol) was added N,N-diisopropylethylamine (0.03611 mL, 0.0002073 mol). The reaction was stirred at rt for 2 h, then quenched with water. The mixture was extracted with ethyl acetate. The combined organic layers were washed with brine, dried and concentrated to dry. The residue was used directly in next step. MS (ESI): (M+H)+=404.2.

出典