Hydrochloric Acid → HCID 70069846, compound

HRID 1289487Notes

Reaction equation

HRID 1289487 reaction equation
[CH2:1]([O:3][C:4]([C@@H:6]1[CH2:11][C:10]([CH3:12])=[CH:9][CH2:8][N:7]1C(OC(C)(C)C)=O)=[O:5])[CH3:2].[ClH:20]>C(OCC)(=O)C>[ClH:20].[CH2:1]([O:3][C:4]([C@@H:6]1[CH2:11][C:10]([CH3:12])=[CH:9][CH2:8][NH:7]1)=[O:5])[CH3:2]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 54234952HCID 54234952, compound

Product 1

HCID 70069846HCID 70069846, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

A stirred, ice-cooled solution of the product from (g) above (3.13 g, 11.62 mmol) in ethyl acetate (30 ml) was saturated with hydrogen chloride over 0.5 hour and then stood at room temperature for a further 2 hours. The solvent was evaporated under reduced pressure and the residue crystallised from a mixture of ether and ethanol to afford the title compound (2.20 g) as white crystals, m.p. 108°-109° C. Rf 0.35 (SS 3), [α]D25 -106.5° (c=1.0, CH3CH2OH). Found: C,52.49; H,7.90; N,6.70. C9H15NO2 ; HCl requires C,52.55; H,7.84; N,6.81%.

Workup

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue crystallised from a mixture of ether and ethanol

Sources & evidence

ORD record
ord-69031e8811c9429698534fcba54cf0d3
Source dataset
uspto-grants-1998_05
Patent number
US05750520

Reaction notes

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