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Hydrochloric Acid → 4-(1,3-Benzodioxol-5-yl)piperidin-4-ol

HRID 1576665
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HRID 1576665 반응식
C([N:8]1[CH2:13][CH2:12][C:11]([OH:23])([C:14]2[CH:19]=[CH:18][C:17]3[O:20][CH2:21][O:22][C:16]=3[CH:15]=2)[CH2:10][CH2:9]1)C1C=CC=CC=1.Cl>[Pd].CO>[OH:23][C:11]1([C:14]2[CH:19]=[CH:18][C:17]3[O:20][CH2:21][O:22][C:16]=3[CH:15]=2)[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 221280344-(2H-1,3-Benzodioxol-5-yl)-1-benzylpiperidin-4-ol

생성물 1

HCID 150347154-(1,3-Benzodioxol-5-yl)piperidin-4-ol

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

39.4 g. 1-benzyl-4-hydroxy-4-(3.4-methylene dioxy phenyl)-piperidine are dissolved in 400 ml. methanol and the solution is mixed with 30 ml. 4-N hydrochloric acid. To this mixture is then added 3 g. of a palladium/carbon catalyst which has been suspended in 60 ml. alcohol. The mixture is hydrogenized at 35° - 40°C under normal pressure. After 3300 ml. hydrogen has been absorbed, hydrogenation is stopped and the cataylst is removed from the mixture by filtering. The mother liquor is heavily concentrated and the 4-hydroxy-4-(3.4-methylene dioxy phenyl)-piperidine hydrochloride with a melting point of 198° - 200°C crystallizes out.

후처리

  1. additionTo this mixture is then added 3 g
  2. customis hydrogenized at 35° - 40°C under normal pressure
  3. customhydrogen has been absorbed
  4. customthe cataylst is removed from the mixture
  5. filtrationby filtering
  6. concentrationThe mother liquor is heavily concentrated
  7. customthe 4-hydroxy-4-(3.4-methylene dioxy phenyl)-piperidine hydrochloride with a melting point of 198° - 200°C crystallizes out

출처 및 근거

ORD 기록
ord-89166f60b9bf43cc8968d0cdaad1fb37
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03982001

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