反応 #89751

反応方程式

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

反応条件

後処理

1. 1
   その他After quenched with water
2. 2
   抽出the mixture was extracted with ethyl acetate
3. 3
   洗浄The combine organic lyers were washed with brine
4. 4
   その他dried
5. 5
   濃縮concentrated
6. 6
   その他to dry
7. 7
   その他The residue was used directly in next step without further purification

実験手順

To a mixture of (2S,3S,5S)-5-methoxy-3-(methoxycarbonyl)piperidine-2-carboxylic acid (14.0 mg, 0.0000644 mol), 1-phenyl-piperazine (0.01231 mL, 8.056E-5 mol) and benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (35.63 mg, 8.056E-5 mol) in N,N-dimethylformamide (0.20 mL, 0.0026 mol) was added N,N-diisopropylethylamine (0.01403 mL, 8.056E-5 mol). The mixture was stirred at rt for 2 h. After quenched with water, the mixture was extracted with ethyl acetate. The combine organic lyers were washed with brine, dried and concentrated to dry. The residue was used directly in next step without further purification. MS (ESI): (M+H)+=362.1.

出典