Dichloromethane → Ethyl 3,4,4-trimethoxypiperidine-1-carboxylate

反応式

[CH3:1][O:2][CH:3]1[C:8]([O:11][CH3:12])([O:9][CH3:10])[CH2:7][CH2:6][NH:5][CH2:4]1.C(Cl)Cl.Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18].C(N(CC)CC)C>>[CH3:1][O:2][CH:3]1[C:8]([O:11][CH3:12])([O:9][CH3:10])[CH2:7][CH2:6][N:5]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:4]1

参加物

反応物 4

HCID 6344Dichloromethane

HCID 8471Triethylamine

HCID 10928Ethyl chloroformate

HCID 198835163,4,4-Trimethoxypiperidine

生成物 1

HCID 3019431Ethyl 3,4,4-trimethoxypiperidine-1-carboxylate

実験手順

The title compound was prepared by taking 3,4,4-trimethoxypiperidine (150 mg, 0.00086 mol) in Methylene chloride (10 mL, 0.2 mol) and adding Ethyl chloroformate (0.098 mL, 0.0010 mol) and Triethylamine (0.24 mL, 0.0017 mol). The reaction was stirred overnight and then quenched with NaHCO3. The crude was obtained by evaporating the organic layer and was taken to the next step as-is (210 mg, 99%). MS calculated for C11H21NO5: (M+H) 248; found 248.1.