Hydrochloric Acid → HCID 68004077, compound

HRID 1896930Notes

Reaction equation

HRID 1896930 reaction equation
O1[C:5]2([CH2:10][CH2:9][CH:8]([CH:11]([NH:14][C:15]([NH:17][CH3:18])=[O:16])[CH2:12][CH3:13])[CH2:7][CH2:6]2)[O:4]CC1.Cl.C(=O)([O-])[O-].[K+].[K+]>CC#N>[CH3:18][NH:17][C:15]([NH:14][CH:11]([CH:8]1[CH2:7][CH2:6][C:5](=[O:4])[CH2:10][CH2:9]1)[CH2:12][CH3:13])=[O:16]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 68003779HCID 68003779, compound

Product 1

HCID 68004077HCID 68004077, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

Into a 50 mL round-bottom flask was placed a solution of 1-(1-1,4-dioxaspiro[4.5]decan-8-ylpropyl)-3-methylurea (as prepared in the previous step, 48 mg, 0.19 mmol, 1.00 equiv) in CH3CN (2 mL), hydrogen chloride (aq, 2M) (2 mL). The resulting solution was stirred for 2 h at room temperature. The pH value of the solution was adjusted to 8 with potassium carbonate (1 mol/L). The resulting solution was extracted with 3×10 mL of dichloromethane. The organic layers were combined, dried over anhydrous sodium sulfate and concentrated under vacuum. The title compound was obtained as a yellow solid.

Workup

  1. customInto a 50 mL round-bottom flask was placed
  2. extractionThe resulting solution was extracted with 3×10 mL of dichloromethane
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under vacuum

Sources & evidence

ORD record
ord-3cbd9502c62f4717a17a0c60054b1020
Source dataset
uspto-grants-2013_08
Patent number
US08518969B2

Reaction notes

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