1,4-Dioxane hydrochloride → HCID 86754545, compound
Reaction equation
[ClH:1].O1CCOCC1.[N:8]1[CH:13]=[CH:12][C:11]([NH:14][C:15](=[O:34])[C:16]2[CH:21]=[CH:20][C:19]([CH2:22][NH:23]C(OC(C)(C)C)=O)=[CH:18][C:17]=2[O:31][CH2:32][CH3:33])=[CH:10][CH:9]=1>>[ClH:1].[ClH:1].[N:8]1[CH:13]=[CH:12][C:11]([NH:14][C:15](=[O:34])[C:16]2[CH:21]=[CH:20][C:19]([CH2:22][NH2:23])=[CH:18][C:17]=2[O:31][CH2:32][CH3:33])=[CH:10][CH:9]=1Participants
3
Procedure
4N Hydrochloric acid-dioxane (1 ml) was added to N-(4- pyridyl)-4-tert-butoxycarbonylaminomethyl-2-ethoxybenzamide (60 mg), and the mixture was stirred at room temperature for 1 hour. After the reaction, the solvent was evaporated under reduced pressure. The obtained crystals were recrystallized from methanol-ethyl acetate to give 40 mg of N-(4- pyridyl)-4-aminomethyl-2-ethoxybenzamide dihydrochloride 1/2 hydrate having a melting point of 251° C. (dec.).
Workup
- customAfter the reaction
- customthe solvent was evaporated under reduced pressure
- customThe obtained crystals were recrystallized from methanol-ethyl acetate
Sources & evidence
- ORD record
- ord-f6414f6f00484356be50b6eb2e440ac4
- Source dataset
- uspto-grants-2000_12
- Patent number
- US06156766
Reaction notes
Loading…