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Hydrochloric Acid → HCID 19424032, compound

HRID 743316
Notes
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Reaction equation

HRID 743316 reaction equation
[ClH:1].[CH3:2][N:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[CH2:8][CH2:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[CH2:17][CH2:18][C:19]1[CH:24]=[C:23]([O:25][CH3:26])[C:22]([O:27][CH3:28])=[C:21]([O:29][CH3:30])[CH:20]=1>O1CCOCC1>[ClH:1].[CH3:2][N:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[CH2:8][CH2:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[CH2:17][CH2:18][C:19]1[CH:20]=[C:21]([O:29][CH3:30])[C:22]([O:27][CH3:28])=[C:23]([O:25][CH3:26])[CH:24]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 19423984HCID 19423984, compound

Product 1

HCID 19424032HCID 19424032, compoundYield 77%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.84 ml of a 4N solution of hydrogen chloride in dioxane was added to a solution of 0.900 g of 1-methyl-2-(2-{2-[2-(3,4,5-trimethoxyphenyl)ethyl]phenoxy}ethyl)pyrrolidine [prepared as described in step (a) above] in a suitable amount of dioxane, and the resulting solution was freed from the solvent by distillation under reduced pressure. The resulting solid was then dissolved in a small amount of methylene chloride, and ethyl acetate was added to the solution, which was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 0.755 g (yield 77%) of the title compound as colorless crystals, melting at 130°-131° C.

Workup

  1. distillationthe resulting solution was freed from the solvent by distillation under reduced pressure
  2. dissolutionThe resulting solid was then dissolved in a small amount of methylene chloride, and ethyl acetate
  3. additionwas added to the solution, which
  4. customto stand at room temperature
  5. customThe crystals which precipitated
  6. filtrationwere collected by filtration
  7. customdried in vacuo

Sources & evidence

ORD record
ord-4ff5accee019451d855e74bc0e6801d6
Source dataset
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05556864

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes