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Water → 3-(3,4-Dimethoxyphenyl)-1-ethylpiperidine

HRID 616029
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HRID 616029 반응식
[C:1]([N:4]1[CH2:9][CH2:8][CH2:7][CH:6]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=2)[CH2:5]1)(=O)[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)(=O)C.O>O1CCCC1>[CH2:1]([N:4]1[CH2:9][CH2:8][CH2:7][CH:6]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=2)[CH2:5]1)[CH3:2]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 203708461-[3-(3,4-Dimethoxyphenyl)piperidin-1-yl]ethan-1-oneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 203708473-(3,4-Dimethoxyphenyl)-1-ethylpiperidine수율 93.2%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

반응 조건

온도
5 °C

실험 절차

A solution of 680 mg of N-acetyl-3-(3',4'-dimethoxyphenyl)-piperidine in 10 ml of tetrahydrofouran was slowly added with stirring at 20° C to 200 mg of lithium aluminum hydride in 10 ml of tetrahydrofuran and the mixture was stirred for an hour and then cooled to 5° C. 10 ml of ethyl acetate were slowly added thereto and the mixture was poured into water and filtered. The aqueous phase was recovered by decanting and was extracted again with ethyl acetate. The combined organic phases were washed with water, dried and evaporated to dryness to obtain 600 mg of N-ethyl-3-(3',4'-dimethoxyphenyl)-piperidine melting at about 50° C.

후처리

  1. filtrationfiltered
  2. customThe aqueous phase was recovered
  3. customby decanting
  4. extractionwas extracted again with ethyl acetate
  5. washThe combined organic phases were washed with water
  6. customdried
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-92cbfc9bcd35494cbcbdb3676827e647
출처 데이터셋
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04072685

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