Potassium Carbonate → HCID 54077540, compound

HRID 1940203Notes

Reaction equation

HRID 1940203 reaction equation
[CH2:1]([O:3][C:4](=[O:32])[CH:5]=[CH:6][C:7](=[O:31])[N:8]([C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=1[CH:21]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[Cl:30])[CH2:22][OH:23])[CH2:9][C:10]([CH3:13])([CH3:12])[CH3:11])[CH3:2].C1OCCOCCOCCOCCOCCOC1.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH2:1]([O:3][C:4](=[O:32])[CH2:5][CH:6]1[O:23][CH2:22][CH:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=2[Cl:30])[C:15]2[CH:16]=[C:17]([Cl:20])[CH:18]=[CH:19][C:14]=2[N:8]([CH2:9][C:10]([CH3:13])([CH3:12])[CH3:11])[C:7]1=[O:31])[CH3:2]

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 70275621HCID 70275621, compound

Product 1

HCID 54077540HCID 54077540, compoundYield 24.1%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To dichloromethane (70 ml) were added 3-[N-[2-[1-(2-chlorophenyl)-2-hydroxyethyl]-4-chlorophenyl]-N-neopentylcarbamoyl]acrylic acid ethyl ester (6.8 g), 18-crown-6 (3.78 g) and potassium carbonate. The mixture was stirred for 3 days at room temperature. Insolubles were filtered off, then the solvent was distilled off. The residue was purified by means of a silica-gel column chromatography (hexane:acetic acid ethyl ester=5:1 v/v as an eluent) to give 1.64 g of a non-crystalline solid product.

Workup

  1. filtrationInsolubles were filtered off
  2. distillationthe solvent was distilled off
  3. customThe residue was purified by means of a silica-gel column chromatography (hexane

Sources & evidence

ORD record
ord-f042136dceae4a228f44f3b0a3288119
Source dataset
uspto-grants-1997_12
Patent number
US05698691

Reaction notes

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