HCID 68977387, compound → HCID 68841554, compound

HRID 1948599Notes

Reaction equation

HRID 1948599 reaction equation
Cl.[O:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11]3([N:21]([CH3:23])[CH3:22])[CH2:20][CH2:19][C:14]4(OCC[O:15]4)[CH2:13][CH2:12]3)=[CH:10][C:5]=2[O:4][CH2:3]1>Cl>[O:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11]3([N:21]([CH3:23])[CH3:22])[CH2:12][CH2:13][C:14](=[O:15])[CH2:19][CH2:20]3)=[CH:10][C:5]=2[O:4][CH2:3]1

Participants

3

Reactant 1

HCID 68977387HCID 68977387, compound

Product 1

HCID 68841554HCID 68841554, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

6N hydrochloric acid (10 ml) was added to (8-benzo[1,3]dioxol-5-yl-1,4-dioxa-spiro[4.5]dec-8-yl)-dimethylamine hydrochloride (2.70 g, 7.91 mmole) and stirred overnight at RT. After completion of the hydrolysis the reaction mixture was extracted with ether (2×20 ml), the aqueous solution was made alkaline with 5N sodium hydroxide solution while cooling with ice, the reaction mixture was extracted with dichloromethane (3×50 ml), and the organic phase was dried over sodium sulfate and concentrated by evaporation in vacuo.

Workup

  1. customAfter completion of the hydrolysis the reaction mixture
  2. extractionwas extracted with ether (2×20 ml)
  3. temperaturewhile cooling with ice
  4. extractionthe reaction mixture was extracted with dichloromethane (3×50 ml)
  5. dry with materialthe organic phase was dried over sodium sulfate
  6. concentrationconcentrated by evaporation in vacuo

Sources & evidence

ORD record
ord-ddaef548f35d481683ad8d89c7693dc9
Source dataset
uspto-grants-2013_03
Patent number
US08399503B2

Reaction notes

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