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Acetone → 1-[4-(p-Fluorophenyl)-4-hydroxy-2-butenyl]-4-(p-chlorophenyl)-4-hydroxypiperidine

HRID 596948
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인쇄 미리보기

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HRID 596948 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]1[CH:13]=[CH:12][C:11]([CH:14]([OH:32])[C:15]#[C:16][CH2:17][N:18]2[CH2:23][CH2:22][C:21]([C:25]3[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=3)([OH:24])[CH2:20][CH2:19]2)=[CH:10][CH:9]=1.CC(C)=O>CCOCC>[F:7][C:8]1[CH:9]=[CH:10][C:11]([CH:14]([OH:32])[CH:15]=[CH:16][CH2:17][N:18]2[CH2:19][CH2:20][C:21]([C:25]3[CH:26]=[CH:27][C:28]([Cl:31])=[CH:29][CH:30]=3)([OH:24])[CH2:22][CH2:23]2)=[CH:12][CH:13]=1
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참가 물질

5

반응물 3

HCID 180AcetoneHCID 132773661-[4-(p-Fluorophenyl)-4-hydroxy-2-butynyl]-4-(p-chlorophenyl)-4-hydroxypiperidineHCID 21226445Aluminium lithium hydride

생성물 1

HCID 536616361-[4-(p-Fluorophenyl)-4-hydroxy-2-butenyl]-4-(p-chlorophenyl)-4-hydroxypiperidine수율 124.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
25 °C

실험 절차

To an ethereal solution (14 ml) of lithium aluminum hydride (0.37 g) was added a solution of 1-[4-(p-fluorophenyl)-4-hydroxy-2-butynyl]-4-(p-chlorophenyl)-4-hydroxypiperidine (1.20 g) in ether (13 ml) under ice-cooling. After stirring at 10° C for 1.5 hours and further at 25° C for 4 hours, acetone was added thereto in order to consume excess of lithium aluminum hydride. The resulting mixture was poured into an aqueous ammonium chloride solution and extracted with ethyl acetate. The ethyl acetate extracts were washed with water, dried over anhydrous magnesium sulfate and concentrated to afford 1-[4-(p-fluorophenyl)-4-hydroxy-2-butenyl]-4-(p-chlorophenyl)-4-hydroxypiperidine (1.50 g) as white needles, M.P. 149° - 151° C.

후처리

  1. temperaturecooling
  2. customin order to consume excess of lithium aluminum hydride
  3. additionThe resulting mixture was poured into an aqueous ammonium chloride solution
  4. extractionextracted with ethyl acetate
  5. washThe ethyl acetate extracts were washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2a182c0a3181448c955cfcd64ba5e69e
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04012515

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