HCID 68697439, compound → HCID 68693412, compound

HRID 1951762Notes

Reaction equation

HRID 1951762 reaction equation
[CH:1]1([CH2:6][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)[CH2:5][CH2:4][CH2:3][CH2:2]1>S(=O)(=O)(O)O>[CH:1]1([CH2:6][C:7]2([N:17]([CH3:18])[CH3:19])[CH2:8][CH2:9][C:10](=[O:11])[CH2:15][CH2:16]2)[CH2:2][CH2:3][CH2:4][CH2:5]1

Participants

3

Reactant 1

HCID 68697439HCID 68697439, compound

Product 1

HCID 68693412HCID 68693412, compound

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Procedure

5% sulfuric acid (600 ml) was added at room temperature to (8-cyclopentylmethyl-1,4-dioxa-spiro[4.5]dec-8-yl)-dimethyl-amine (13.4 g, 50 mmol), and the mixture was stirred for 3 d at RT. The reaction mixture was extracted with ether (2×50 ml). Then the aqueous phase was rendered alkaline with 5N NaOH, while cooling with an ice bath, and extraction with dichloromethane (3×50 ml) was carried out. The organic phase was dried over Na2SO4 and concentrated to dryness in vacuo.

Workup

  1. extractionThe reaction mixture was extracted with ether (2×50 ml)
  2. temperaturewhile cooling with an ice bath
  3. extractionextraction with dichloromethane (3×50 ml)
  4. dry with materialThe organic phase was dried over Na2SO4
  5. concentrationconcentrated to dryness in vacuo

Sources & evidence

ORD record
ord-1c20132a6a4d40ba96d9769ecde04876
Source dataset
uspto-grants-2013_03
Patent number
US08404740B2

Reaction notes

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