Potassium Carbonate → HCID 22370982, compound

HRID 2294117Notes

Reaction equation

HRID 2294117 reaction equation
Cl.Cl.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][CH2:19][NH:20][C:21]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:22])[CH2:13][CH2:12]1.C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C>[CH3:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][CH2:19][NH:20][C:21]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:22])[CH2:15][CH2:16]1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 22371062HCID 22371062, compound

Product 1

HCID 22370982HCID 22370982, compoundYield 96.2%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

A mixture of benzyl 3-[4-(2-methoxyphenyl)piperazin-1-yl]propylamino-formate dihydrochloride (481 g, 1.05 mol) and potassium carbonate (630 mL, 5.5N, 3.15 mol) in 4L of ethyl acetate was stirred at room temperature for 1 hour. The mixture was washed with water (1×630 mL), treated with silica gel (200 g) and filtered. The filtrate was concentrated under reduced pressure to give benzyl 3-[4-(2-methoxyphenyl)piperazin-1-yl]propylaminoformate (385.9 g, 1.01 mol) as an oil.

Workup

  1. washThe mixture was washed with water (1×630 mL)
  2. additiontreated with silica gel (200 g)
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-db76b986ff0a4effa2e27fe87d3e88e0
Source dataset
uspto-grants-1997_11
Patent number
US05688795

Reaction notes

Loading…