Ethanol hydrochloride → HCID 68926984, compound

HRID 385692Notes

Reaction equation

HRID 385692 reaction equation
[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8](=[O:32])[N:9]2[CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][CH:17]([NH:20][CH2:21][C:22]3[N:27]=[CH:26][C:25]4[O:28][CH2:29][CH2:30][O:31][C:24]=4[CH:23]=3)[CH2:16][CH2:15]2)=[N:4][CH:3]=1.[ClH:33].C(O)C>C(O)C.C(OCC)(=O)C>[ClH:33].[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8](=[O:32])[N:9]2[CH2:12][CH2:13][N:14]2[CH2:15][CH2:16][CH:17]([NH:20][CH2:21][C:22]3[N:27]=[CH:26][C:25]4[O:28][CH2:29][CH2:30][O:31][C:24]=4[CH:23]=3)[CH2:18][CH2:19]2)=[N:4][CH:3]=1

Participants

5

Reactant 2

HCID 21887872Ethanol hydrochlorideHCID 57815413HCID 57815413, compound

Product 1

HCID 68926984HCID 68926984, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

To a solution of 0.095 g of 7-amino-1-(2-(4-((2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)amino)piperidin-1-yl)ethyl)-1,5-naphthyridin-2(1H)-one in 3 mL of ethanol and 2 mL of ethyl acetate, 4 mL of a 2 mol/L hydrogen chloride/ethanol solution was added at room temperature, and the mixture was stirred at room temperature for 20 minutes, and the solvent was distilled off under reduced pressure. To the residue, 8 mL of diethyl ether was added, the residue was suspended therein, and the solid was filtered off to obtain 0.41 g of 7-amino-1-(2-(4-((2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)amino)piperidin-1-yl)ethyl)-1,5-naphthyridin-2(1H)-one hydrochloride as a yellow solid.

Workup

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionTo the residue, 8 mL of diethyl ether was added
  3. filtrationthe solid was filtered off

Sources & evidence

ORD record
ord-126cf065c06c425ebeac59261ea1b872
Source dataset
uspto-grants-2013_02
Patent number
US08367831B2

Reaction notes

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