HCID 68841469, compound → HCID 68694413, compound

HRID 1948610Notes

Reaction equation

HRID 1948610 reaction equation
Cl.[CH2:2]([C:4]1([N:14]([CH3:16])[CH3:15])[CH2:13][CH2:12][C:7]2(OCC[O:8]2)[CH2:6][CH2:5]1)[CH3:3]>Cl>[CH3:15][N:14]([CH3:16])[C:4]1([CH2:2][CH3:3])[CH2:13][CH2:12][C:7](=[O:8])[CH2:6][CH2:5]1

Participants

3

Reactant 1

HCID 68841469HCID 68841469, compound

Product 1

HCID 68694413HCID 68694413, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

(8-ethyl-1,4-dioxa-spiro[4.5]dec-8-yl)-dimethylamine hydrochloride (6.67 g, 0.026 mmole) was dissolved in 6N HCl (40 ml) and stirred overnight at room temperature. The reaction mixture was extracted twice with diethyl ether (100 ml). The reaction mixture was then made alkaline with 5N NaOH while cooling with ice and extracted a further three times with Et2O (100 ml). The combined organic phases were dried over Na2SO4, filtered, and the solvent was removed in vacuo.

Workup

  1. extractionThe reaction mixture was extracted twice with diethyl ether (100 ml)
  2. temperaturewhile cooling with ice
  3. extractionextracted a further three times with Et2O (100 ml)
  4. dry with materialThe combined organic phases were dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo

Sources & evidence

ORD record
ord-445d560e766b4c92bbfad8705a355321
Source dataset
uspto-grants-2013_03
Patent number
US08399503B2

Reaction notes

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