Methanol → Methyl 4-aminopiperidine-4-carboxylate dihydrochloride

반응식

[ClH:1].Cl.[NH2:3][C:4]1([C:10]([OH:12])=[O:11])[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[CH3:13]O>>[ClH:1].[ClH:1].[NH2:3][C:4]1([C:10]([O:12][CH3:13])=[O:11])[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1

참가 물질

반응물 2

HCID 887Methanol

HCID 229070884-Aminopiperidine-4-carboxylic acid--hydrogen chloride (1/2)

생성물 1

HCID 22907214Methyl 4-aminopiperidine-4-carboxylate dihydrochloride

실험 절차

Into a heterogeneous mixture of 4-amino-4-carboxypiperidine dihydrochloride (61.0 g, 0.34 mmol) in methanol (600 mL) is bubbled hydrogen chloride gas at room temperature. The reaction mixture is concentrated to dryness in vacuo, dissolved in 1,4-dioxane (200 mL), and concentrated in vacuo. The residue is redissolved in methanol (1600 mL) into which hydrogen chloride gas is bubbled for 45 minutes. The reaction mixture is refluxed for 18 hours. Most of the solvent is then evaporated, the product is collected by filtration, and washed with ethyl acetate to give 4-amino-4-carbomethoxypiperidine dihydrochloride.

후처리

customis bubbled hydrogen chloride gas at room temperature
concentrationThe reaction mixture is concentrated to dryness in vacuo
dissolutiondissolved in 1,4-dioxane (200 mL)
concentrationconcentrated in vacuo
dissolutionThe residue is redissolved in methanol (1600 mL) into which hydrogen chloride gas
customis bubbled for 45 minutes
temperatureThe reaction mixture is refluxed for 18 hours
customMost of the solvent is then evaporated
filtrationthe product is collected by filtration
washwashed with ethyl acetate

출처 및 근거

ORD 기록: ord-3694f89379a941b8b090c9220f1ff57a
출처 데이터셋: uspto-grants-1997_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05646167

반응 노트

불러오는 중…