Hydrochloric Acid → HCID 20380002, compound

HRID 1448495Notes

Reaction equation

HRID 1448495 reaction equation
[ClH:1].O[C:3]([CH:16]1[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][CH2:24][C:25]([C:27]2[S:28][CH:29]=[CH:30][CH:31]=2)=[O:26])[CH2:18][CH2:17]1)([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl>C(O)(C)C>[ClH:1].[C:4]1([C:3]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[C:16]2[CH2:17][CH2:18][N:19]([CH2:22][CH2:23][CH2:24][C:25]([C:27]3[S:28][CH:29]=[CH:30][CH:31]=3)=[O:26])[CH2:20][CH2:21]2)[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

Participants

4

Conditions

Temperature
80 °C

Procedure

A mixture of 22.8 g (0.05 mole) of 4-[4-(α-hydroxy-α-phenylbenzyl)piperidino]-1-(2-thienyl)butan-1-one hydrochloride, 500 ml of isopropyl alcohol and 500 ml of concentrated HCl was heated on a steam bath for 3 hours, and the solvent was removed under vacuum. Isopropyl alcohol and 300 ml of water were added to the residue and heated to 80° C. Upon cooling a precipitate formed which was collected and recrystallized from methanol-ethyl acetate and toluene to give the desired product, M.P. 132.5°-134.5° C.

Workup

  1. temperaturewas heated on a steam bath for 3 hours
  2. customthe solvent was removed under vacuum
  3. additionIsopropyl alcohol and 300 ml of water were added to the residue
  4. temperatureUpon cooling a precipitate
  5. customformed which
  6. customwas collected
  7. customrecrystallized from methanol-ethyl acetate and toluene

Sources & evidence

ORD record
ord-5ba510d4c78d4654a3c469dfe61c4c7f
Source dataset
uspto-grants-1979_12
Patent number
US04180583

Reaction notes

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