HCID 22923955, compound → HCID 22923961, compound

HRID 2258000Notes

Reaction equation

HRID 2258000 reaction equation
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][C:8]([C:20]([O:22][CH2:23][CH3:24])=[O:21])([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9][C:10]([O:12]CC)=[O:11])=[CH:3][CH:2]=1>Cl>[N:1]1[CH:2]=[CH:3][C:4]([CH2:7][C:8]([C:20]([O:22][CH2:23][CH3:24])=[O:21])([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9][C:10]([OH:12])=[O:11])=[CH:5][CH:6]=1

Participants

3

Reactant 1

HCID 22923955HCID 22923955, compound

Product 1

HCID 22923961HCID 22923961, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

8.75 g of ethyl 4-(4-pyridyl)-3,3-bisethoxycarbonylbutyrate are stirred at 50°-60° C. in 500 ml of 6N HCl for 2 h. The mixture is then concentrated in vacuo and allowed to react again at 50°-60° C. with 500 ml of 6N HCl for 2 h. It is then concentrated to dryness in vacuo and redistilled twice using a little toluene. The residue is taken up in a little water and freeze-dried.

Workup

  1. concentrationThe mixture is then concentrated in vacuo
  2. customto react again at 50°-60° C. with 500 ml of 6N HCl for 2 h
  3. concentrationIt is then concentrated to dryness in vacuo
  4. distillationredistilled twice
  5. customfreeze-dried

Sources & evidence

ORD record
ord-bbb2146228c64503abb629fec732128c
Source dataset
uspto-grants-1997_08
Patent number
US05658935

Reaction notes

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