反応 #89756

反応方程式

methyl chloroformate

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

methylene chloride

→

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

反応条件

後処理

1. 1
   その他After quenched with aq. sodium bicaronate
2. 2
   抽出the reaction 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 methyl(2S,3S,5S)-5-tert-butoxy-2-[(4-phenylpiperazin-1-yl)carbonyl]piperidine-3-carboxylate (0.03345 g, 8.290E-5 mol) and 4-dimethylaminopyridine (0.0152 g, 0.000124 mol) in methylene chloride (1.50 mL, 0.0234 mol) was added methyl chloroformate (0.00833 mL, 0.000108 mol). The reaction was stirred at rt overnight. After quenched with aq. sodium bicaronate, the reaction was extracted with ethyl acetate. The combined organic layers were washed with brine, dried, concentrated to dry. The resulting residue was used directly in next step. MS (ESI): (M+H)+=462.2.

出典