Hydrochloric Acid → HCID 19787938, compound

HRID 1656343Notes

Reaction equation

HRID 1656343 reaction equation
O1[C:5]2([CH2:10][CH2:9][N:8]([C:11]3[N:16]=[C:15]([C:17]([NH2:19])=[O:18])[CH:14]=[CH:13][N:12]=3)[CH2:7][CH2:6]2)[O:4]CC1.Cl>C(O)(=O)C>[O:4]=[C:5]1[CH2:10][CH2:9][N:8]([C:11]2[N:16]=[C:15]([C:17]([NH2:19])=[O:18])[CH:14]=[CH:13][N:12]=2)[CH2:7][CH2:6]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 19787950HCID 19787950, compound

Product 1

HCID 19787938HCID 19787938, compoundYield 87.9%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture of 4.1 g (0.0155 mol) of 2-(1,4-dioxa-8-azaspiro[4.5]decan-8-yl]pyrimidine-4-carboxamide, 41 ml of acetic acid and 4.1 ml of concentrated hydrochloric acid is heated at reflux temperature for 30 minutes. The mixture is concentrated under reduced pressure, the residue is then taken up in a mixture of dichloromethane and water, is alkalified with aqueous ammonia solution, extracted with dichloromethane, the organic phase is dried over magnesium sulphate, filtered and the solvent evaporated under reduced pressure. 3 g of compound are obtained.

Workup

  1. temperatureis heated
  2. temperatureat reflux temperature for 30 minutes
  3. concentrationThe mixture is concentrated under reduced pressure
  4. additionthe residue is then taken up in a mixture of dichloromethane and water
  5. extractionextracted with dichloromethane
  6. dry with materialthe organic phase is dried over magnesium sulphate
  7. filtrationfiltered
  8. customthe solvent evaporated under reduced pressure

Sources & evidence

ORD record
ord-42343e72e91c450282638d25dbf947ec
Source dataset
uspto-grants-1993_10
Patent number
US05254560

Reaction notes

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