Hydrochloric Acid → HCID 57475101, compound
Reaction equation
Cl.[S:2]1[C:6]([C:7]2([N:17]([CH3:19])[CH3:18])[CH2:16][CH2:15][C:10]3(OCC[O:11]3)[CH2:9][CH2:8]2)=[CH:5][C:4]2[CH:20]=[CH:21][CH:22]=[CH:23][C:3]1=2.Cl.CNC.Cl>O>[S:2]1[C:6]([C:7]2([N:17]([CH3:18])[CH3:19])[CH2:16][CH2:15][C:10](=[O:11])[CH2:9][CH2:8]2)=[CH:5][C:4]2[CH:20]=[CH:21][CH:22]=[CH:23][C:3]1=2Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
The 8-benzo[b]thiophen-2-yl-1,4-dioxa-spiro[4.5]dec-8-yl)-dimethylamine hydrochloride (0.60 g, 1.7 mmole) was dissolved in water (0.8 ml), conc. hydrochloric acid (1.04 ml, 151 mmole) was added, and the mixture was stirred for 3 days at room temperature. After completion of the hydrolysis the reaction mixture was extracted with diethyl ether (2×25 ml) and the aqueous phase was made alkaline with 5N sodium hydroxide solution, extracted with dichloromethane (3×25 ml), dried over sodium sulfate and concentrated by evaporation in vacuo.
Workup
- customAfter completion of the hydrolysis the reaction mixture
- extractionwas extracted with diethyl ether (2×25 ml)
- extractionextracted with dichloromethane (3×25 ml)
- dry with materialdried over sodium sulfate
- concentrationconcentrated by evaporation in vacuo
Sources & evidence
- ORD record
- ord-855cf426a089495aabfe230ebc82b991
- Source dataset
- uspto-grants-2013_03
- Patent number
- US08399503B2
Reaction notes
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