Hydrogen chloride-ethyl acetate → HCID 23082084, compound
Reaction equation
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[NH:15][C:16](=[O:24])[C:17]3[C:22]([CH:23]=2)=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:10][CH:9]1[CH2:25][OH:26])=O)(C)(C)C.C(OCC)(=O)C.[ClH:33]>C(OCC)(=O)C>[ClH:33].[OH:26][CH2:25][CH:9]1[CH2:10][CH:11]([C:14]2[NH:15][C:16](=[O:24])[C:17]3[C:22]([CH:23]=2)=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:12][CH2:13][NH:8]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
The obtained 3-(1-t-butoxycarbonyl-2-hydroxymethylpiperidin-4-yl)-2H-isoquinolin-1-one (616 mg) was dissolved in ethyl acetate, and 4N hydrogen chloride-ethyl acetate solution (2.0 ml) was added to the solution, and the mixture was stirred at room temperature for 6.5 hr. The reaction mixture was concentrated, and the precipitated crystals were washed with diethyl ether and dried under reduced pressure to give 3-(2-hydroxymethylpiperidin-4-yl)-2H-isoquinolin-1-one hydrochloride (433 mg).
Workup
- concentrationThe reaction mixture was concentrated
- washthe precipitated crystals were washed with diethyl ether
- customdried under reduced pressure
Sources & evidence
- ORD record
- ord-27d7ba3a70144fb4b62d41a412352aab
- Source dataset
- uspto-grants-2010_10
- Patent number
- US07812178B2
Reaction notes
Loading…