Methanol → HCID 67539285, compound

HRID 39833Notes

Reaction equation

HRID 39833 reaction equation
CO.[O:3]1[C:8]2[CH:9]=[CH:10][C:11]([CH2:13][N:14]([CH:22]3[CH2:27][CH2:26][N:25]([CH2:28][CH2:29][N:30]4[C:39]5[C:34](=[CH:35][CH:36]=[C:37]([C:40]6[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=6)[CH:38]=5)[C:33]([CH3:46])=[CH:32][C:31]4=[O:47])[CH2:24][CH2:23]3)C(=O)OC(C)(C)C)=[CH:12][C:7]=2[O:6][CH2:5][CH2:4]1.[ClH:48].C(OCC)(=O)C>C(OCC)(=O)C>[ClH:48].[O:3]1[C:8]2[CH:9]=[CH:10][C:11]([CH2:13][NH:14][CH:22]3[CH2:23][CH2:24][N:25]([CH2:28][CH2:29][N:30]4[C:39]5[C:34](=[CH:35][CH:36]=[C:37]([C:40]6[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=6)[CH:38]=5)[C:33]([CH3:46])=[CH:32][C:31]4=[O:47])[CH2:26][CH2:27]3)=[CH:12][C:7]=2[O:6][CH2:5][CH2:4]1

Participants

5

Reactant 3

HCID 887Methanol2×HCID 21866389Hydrogen chloride-ethyl acetate2×HCID 59398287HCID 59398287, compound

Product 1

HCID 67539285HCID 67539285, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

To 0.4 mL of methanol solution containing 47 mg of tert-butyl (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)(1-(2-(4-methyl-2-oxo-7-phenylquinolin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate, 0.4 mL of 4 mol/L hydrogen chloride/ethyl acetate solution was added, and stirred for 30 min. 0.8 mL of methanol and 0.8 mL of 4 mol/L hydrogen chloride/ethyl acetate solution were further added, stirred for 2 hours and allowed to stand at room temperature for 13 hours. Ethyl acetate was added, and the resulting solid was filtered to give 34 mg of 1-(2-(4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-4-methyl-7-phenylquinolin-2(1H)-one hydrochloride as a white solid.

Workup

  1. additionwas added
  2. stirringstirred for 2 hours
  3. waitto stand at room temperature for 13 hours
  4. filtrationthe resulting solid was filtered

Sources & evidence

ORD record
ord-3d24366a98184be0a3d51c849257dc9e
Source dataset
uspto-grants-2013_09
Patent number
US08524738B2

Reaction notes

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