Hydrogen chloride-ethyl acetate → HCID 57697530, compound

HRID 1692605Notes

Reaction equation

HRID 1692605 reaction equation
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:8]2[CH:9]=[CH:10][C:11]3[CH2:12][N:13](C(OC(C)(C)C)=O)[CH2:14][CH2:15][O:16][C:17]=3[N:18]=2)[CH2:3]1.Cl.C(OCC)(=O)C>>[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:8]2[CH:9]=[CH:10][C:11]3[CH2:12][NH:13][CH2:14][CH2:15][O:16][C:17]=3[N:18]=2)[CH2:3]1

Participants

3

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 67279637HCID 67279637, compound

Product 1

HCID 57697530HCID 57697530, compoundYield 67%

Procedure

A mixture of the compound (0.15 g) obtained in step 1 and 4N hydrogen chloride/ethyl acetate (2 mL) was stirred at room temperature for 3 hr. The precipitate was collected by filtration, and the aqueous layer was made basic with ethyl acetate and aqueous sodium hydroxide solution. The organic layer was washed with brine and dried, and the solvent was evaporated under reduced pressure. The residue was recrystallized from pentane to give the title compound (0.07 g, 67%) as a white powder.

Workup

  1. filtrationThe precipitate was collected by filtration
  2. washThe organic layer was washed with brine
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was recrystallized from pentane

Sources & evidence

ORD record
ord-433942dfcd754367a38eb2bbc603a3d2
Source dataset
uspto-grants-2012_04
Patent number
US08158617B2

Reaction notes

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