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

HRID 1576665
ノート
印刷プレビュー

反応式

HRID 1576665 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-89166f60b9bf43cc8968d0cdaad1fb37
出典データセット
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03982001

反応ノート

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