HCID 68841469, compound → HCID 68694413, compound
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]1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
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
- extractionThe reaction mixture was extracted twice with diethyl ether (100 ml)
- temperaturewhile cooling with ice
- extractionextracted a further three times with Et2O (100 ml)
- dry with materialThe combined organic phases were dried over Na2SO4
- filtrationfiltered
- 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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