Hydrochloric Acid → HCID 54348121, compound

HRID 2379445Notes

Reaction equation

HRID 2379445 reaction equation
[OH-].[Na+].O.[CH2:4]1[C@@H:9]2[C:10]3[CH:22]=[CH:21][CH:20]=[CH:19][C:11]=3[CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[N:8]2[CH2:7][CH2:6][N:5]1[CH2:23][CH2:24][O:25][CH2:26][C:27]([O:29]CC)=[O:28].Cl>C(O)C>[CH2:4]1[C@@H:9]2[C:10]3[CH:22]=[CH:21][CH:20]=[CH:19][C:11]=3[CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[N:8]2[CH2:7][CH2:6][N:5]1[CH2:23][CH2:24][O:25][CH2:26][C:27]([OH:29])=[O:28]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 86748237HCID 86748237, compound

Product 1

HCID 54348121HCID 54348121, compoundYield 94.4%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

65 ml of a 10% w/v aqueous solution of sodium hydroxide and 200 ml of water were added to a solution of 44.85 g of ethyl (S)-2-(1,2,3,4,10,14b-hexahydrodibenzo[c,f]pyrazino[1,2-a]azepin-2-yl)ethoxyacetate (prepared as described in Example 58) in 450 ml of ethanol, and the mixture was stirred at room temperature for 2 hours. At the end of this time, it was adjusted to a pH value of 4 by the addition of concentrated hydrochloric acid and concentrated by evaporation under reduced pressure. The crystals which precipitated were collected by filtration and recrystallized from water to give 39.20 g (yield 90%) of the title compound as the monohydrate, melting at 105°-108° C.

Workup

  1. concentrationconcentrated by evaporation under reduced pressure
  2. customThe crystals which precipitated
  3. filtrationwere collected by filtration
  4. customrecrystallized from water

Sources & evidence

ORD record
ord-ccfd08abd03a4814bebb01698753727e
Source dataset
uspto-grants-1994_11
Patent number
US05362725

Reaction notes

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