Hydrochloric Acid → HCID 70051991, compound
Reaction equation
[ClH:1].[CH:2]1([C:5]2[O:9]C=[N:7][C:6]=2[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH2:4][CH2:3]1>C(O)C>[ClH:1].[NH2:7][CH:6]([C:5](=[O:9])[CH:2]1[CH2:4][CH2:3]1)[C:10]([O:12][CH2:13][CH3:14])=[O:11]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 50 °C
Procedure
Concentrated hydrochloric acid (21.5 ml) was added to a solution of the product of step (a) (9.3 g) in ethanol (65 ml). The mixture was heated at 50° C. for 1 h, cooled and the solvent was evaporated. Toluene (3×50 ml) was added to the residue and was evaporated after each addition. The residue was triturated with diisopropyl ether (80 ml) to give the title compound (Intermediate 12) as a pale brown powder (6.8 g) m.p. 158°-159° C.
Workup
- temperaturecooled
- customthe solvent was evaporated
- additionToluene (3×50 ml) was added to the residue
- customwas evaporated
- additionafter each addition
- customThe residue was triturated with diisopropyl ether (80 ml)
Sources & evidence
- ORD record
- ord-7de18db56522484fb9af0f1236a12286
- Source dataset
- uspto-grants-1994_07
- Patent number
- US05332831
Reaction notes
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