Hydrochloric Acid → 1-(1,2-Diamino-1-methylethyl)-1-cyclopropanecarboxylate dihydrochloride
Reaction equation
[NH2:1][C:2]([C:6]1([C:9]([O:11]C(C)(C)C)=[O:10])[CH2:8][CH2:7]1)([CH3:5])[CH2:3][NH2:4].O.[ClH:17]>>[ClH:17].[ClH:17].[NH2:1][C:2]([C:6]1([C:9]([OH:11])=[O:10])[CH2:7][CH2:8]1)([CH3:5])[CH2:3][NH2:4]Participants
4
Procedure
0.82 g (3.83 mmol) of the crude tert-butyl 1-(1,2-diamino-1-methyl ethyl)-1-cyclopropanecarboxylate was dissolved in concentrated hydrochloric acid (5 mL) at room temperature, and the solution was stirred at the same temperature for 30 minutes. After adding water to the reaction solution, the solvent was removed by distillation under reduced pressure. The residue was azeotropically distilled with ethanol (twice) to obtain 0.82 g (3.55 mmol, 93%) of the crude target compound as a pale yellow foam solid. The thus obtained crude product was used in the subsequent reaction with no further purification.
Workup
- customthe solvent was removed by distillation under reduced pressure
- distillationThe residue was azeotropically distilled with ethanol (twice)
- customto obtain 0.82 g (3.55 mmol, 93%) of the crude target compound as a pale yellow foam solid
- customThe thus obtained crude product
- customwas used in the subsequent reaction with no further purification
Sources & evidence
- ORD record
- ord-d78f1a5a4ef64d79a5180f81b35c576e
- Source dataset
- uspto-grants-2012_07
- Patent number
- US08211910B2
Reaction notes
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