Hydrochloric Acid → HCID 13106543, compound

HRID 728055Notes

Reaction equation

HRID 728055 reaction equation
[CH3:1][N:2]([CH3:30])[CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([OH:29])[CH:24]=2)(O)[CH:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:14][CH3:15])=[CH:8][CH:7]=1.C(O)C.[ClH:34]>C(Cl)(Cl)Cl.CO>[ClH:34].[CH3:30][N:2]([CH3:1])[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9](/[C:12](/[C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([OH:29])[CH:24]=2)=[C:13](\[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)/[CH2:14][CH3:15])=[CH:10][CH:11]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 13106542HCID 13106542, compound

Product 1

HCID 13106543HCID 13106543, compound

Reagents, catalysts & solvents 1

HCID 21584188Chloroform methanolSolvent

Procedure

40.5 G. (0.1 mole) of the diastereomeric mixture of 1-[4'-(2-dimethylaminoethoxy)phenyl]-1-(3'-hydroxyphenyl)2-phenyl-n-butan-1-ol in 500 ml. ethanol are added to 25 ml. concentrated hydrochloric acid and refluxed for 2 hours. Then the solvent is removed in vacuo and the residue is crystallized from methanol/ ether (1/1). Obtained are colorless crystals having a melting point of 221° C. (dec.); Rf 0.25 [CHCl3 /CH3OH (7/3)]; yield 20.3 g. (48%).

Workup

  1. customThen the solvent is removed in vacuo
  2. customthe residue is crystallized from methanol/ ether (1/1)
  3. customObtained

Sources & evidence

ORD record
ord-1d7ec15eaa80483c83847c7a011528cc
Source dataset
uspto-grants-1991_09
Patent number
US05047431

Reaction notes

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