Piperidine → 2-(2-Nitro-5-piperdinylphenyl)-1,3-dioxolane

HRID 256179

반응식

HRID 256179 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]([N+:13]([O-:15])=[O:14])=[C:6]([CH:8]2[O:12][CH2:11][CH2:10][O:9]2)[CH:7]=1.[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>>[N+:13]([C:5]1[CH:4]=[CH:3][C:2]([N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)=[CH:7][C:6]=1[CH:8]1[O:12][CH2:11][CH2:10][O:9]1)([O-:15])=[O:14]

참가 물질

3

반응물 2

HCID 8082PiperidineHCID 2673852-(5-Chloro-2-nitrophenyl)-1,3-dioxolane

생성물 1

HCID 139875982-(2-Nitro-5-piperdinylphenyl)-1,3-dioxolane수율 100%

실험 절차

A mixture of 2-(5-chloro-2-nitrophenyl)-1,3-dioxolane (21.3 g, 0.09 mole) and piperidine (39.6 g, 0.46 mole) was heated at reflux in an oil bath. After 3 hours, excess piperidine was evaporated and the residue partitioned between water and dichloromethane. The organic phase was separated and the aqueous layer extracted with dichloromethane. Combined extracts were washed with water, dried over magnesium sulfate and concentrated in vacuo to afford 2-(2-nitro-5-piperdinylphenyl)-1,3-dioxolane (21.6 g, 100%) as a dark colored oil which was used without further purification. An analytical sample was purified by flash chromatography using dichloromethane as eluant to give a light yellow oil.

후처리

  1. temperaturewas heated
  2. temperatureat reflux in an oil bath
  3. customexcess piperidine was evaporated
  4. customthe residue partitioned between water and dichloromethane
  5. customThe organic phase was separated
  6. extractionthe aqueous layer extracted with dichloromethane
  7. washCombined extracts were washed with water
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-780747b03da34d5da4302f7cf0abbebe
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04701459

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