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Potassium Hydroxide → 3,4,4-Trimethoxypiperidine

HRID 1088358
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HRID 1088358 반응식
[CH3:1][O:2][CH:3]1[C:8]([O:11][CH3:12])([O:9][CH3:10])[CH2:7][CH2:6][N:5](C(OCC)=O)[CH2:4]1.[OH-].[K+]>CC(O)C>[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 3019431Ethyl 3,4,4-trimethoxypiperidine-1-carboxylate

생성물 1

HCID 198835163,4,4-Trimethoxypiperidine수율 75.4%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
10 °C

실험 절차

A mixture of 117.7 parts of ethyl 3,4,4-tri-methoxy-1-piperidinecarboxylate, 267.3 parts of potassium hydroxide and 720 parts of 2-propanol was stirred and refluxed for 4 hours. The reaction mixture was evaporated. 900 Parts of water were added to the residue and the whole was stirred in a boiling water-bath. The last traces of 2-propanol were removed by evaporation on a Rotavapor. After cooling to 10° C., the product was extracted twice with 280 parts of 1,1'-oxybisethane. The extracts were dried, filtered and evaporated, yielding 62.9 parts (75.4%) of 3,4,4-trimethoxypiperidine as a residue (intermediate 65).

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후처리

  1. temperaturerefluxed for 4 hours
  2. customThe reaction mixture was evaporated
  3. addition900 Parts of water were added to the residue
  4. stirringthe whole was stirred in a boiling water-bath
  5. customThe last traces of 2-propanol were removed by evaporation on a Rotavapor
  6. extractionthe product was extracted twice with 280 parts of 1,1'-oxybisethane
  7. customThe extracts were dried
  8. filtrationfiltered
  9. customevaporated

출처 및 근거

ORD 기록
ord-e53b307993f74395b25becde1225961a
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04962115

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