Hydrogen chloride-ethyl acetate → HCID 23082084, compound

HRID 1352438Notes

Reaction equation

HRID 1352438 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]1

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 23082104HCID 23082104, compound

Product 1

HCID 23082084HCID 23082084, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

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

  1. concentrationThe reaction mixture was concentrated
  2. washthe precipitated crystals were washed with diethyl ether
  3. customdried under reduced pressure

Sources & evidence

ORD record
ord-1e1f12c13666412b828d7b5bcf4e18dd
Source dataset
uspto-grants-2007_05
Patent number
US07220759B2

Reaction notes

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