Hydrochloric Acid → HCID 131710906, compound

HRID 2072467Notes

Reaction equation

HRID 2072467 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[C:8](=[O:14])[CH:7]([CH2:15][N:16]1[CH2:32][CH2:31][C:19]3([N:23]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[CH2:22][NH:21][C:20]3=[O:30])[CH2:18][CH2:17]1)[CH2:6]2.[ClH:33]>O1CCOCC1.CCOCC>[ClH:33].[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[C:8](=[O:14])[CH:7]([CH2:15][N:16]1[CH2:17][CH2:18][C:19]3([N:23]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[CH2:22][NH:21][C:20]3=[O:30])[CH2:31][CH2:32]1)[CH2:6]2

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 21408213HCID 21408213, compound

Product 1

HCID 131710906HCID 131710906, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 312751,4-DioxaneSolvent2×

Procedure

8-[(2,3-Dihydro-5,6-dimethoxy-1-oxo-1H-inden-2-yl)methyl]-1-phenyl-1,3,8-triazaspiro[4.5]decan-4-one (2.75 g) is taken up in 400 ml of boiling dioxane and filtered while hot. The filtrate is concentrated to half its original volume, cooled and treated with 1.2 equivalents of a solution of hydrogen chloride in dioxane. The resulting solution is then diluted with 200 ml of ether and chilled. The crude hydrochloride salt thus obtained is triturated with boiling absolute ethanol (50 ml), cooled and filtered to yield 1.68 g of the title compound, melting point 210°-211° C.

Workup

  1. filtrationfiltered while hot
  2. concentrationThe filtrate is concentrated to half its original volume
  3. temperaturecooled
  4. temperaturechilled
  5. customThe crude hydrochloride salt thus obtained
  6. customis triturated
  7. temperaturecooled
  8. filtrationfiltered

Sources & evidence

ORD record
ord-4b0ab41d1b4049c8862a48780ef4890f
Source dataset
uspto-grants-1977_09
Patent number
US04051248

Reaction notes

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