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Hydrochloric Acid → Ethyl 6-methylpiperidine-3-carboxylate

HRID 1019660
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HRID 1019660 반응식
[CH3:1][CH:2]1[NH:7][CH2:6][CH:5]([C:8]([OH:10])=[O:9])[CH2:4][CH2:3]1.Cl.[OH-].[Na+].[CH3:14][CH2:15]O>O>[CH3:1][CH:2]1[NH:7][CH2:6][CH:5]([C:8]([O:10][CH2:14][CH3:15])=[O:9])[CH2:4][CH2:3]1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 136586116-Methylpiperidine-3-carboxylic acid

생성물 1

HCID 13658605Ethyl 6-methylpiperidine-3-carboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 194.1 (1044 mg, 7.29 mmol) in EtOH (5207 μL) was added concentrated hydrochloric acid (405 μL, 7.29 mmol). The resulting solution was heated at reflux for 18 hours. The reaction mixture was then cooled to room temperature and poured onto water. The reaction was brought to pH 10 with 1N sodium hydroxide in water and was then extracted with EtOAc. The organic phase was then dried over anhydrous Na2SO4 and filtered to provide ethyl 6-methylpiperidine-3-carboxylate. ESI-MS M+H 172.2.

후처리

  1. temperatureThe resulting solution was heated
  2. temperatureat reflux for 18 hours
  3. additionpoured onto water
  4. extractionwas then extracted with EtOAc
  5. dry with materialThe organic phase was then dried over anhydrous Na2SO4
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-0bb690bac5c14fe995633729d8984e73
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716281B2

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