Sodium Bicarbonate → HCID 54350404, compound

HRID 1065786Notes

Reaction equation

HRID 1065786 reaction equation
C1(S(O)(=O)=O)C2C=CC=C(S(O)(=O)=O)C=2C=CC=1.[CH2:19]([O:21][C:22](=[O:42])[C:23]([CH3:41])([CH3:40])[C:24](=[O:39])[CH:25]([O:31][C:32]1[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][CH:33]=1)[N:26]1[CH:30]=[CH:29][N:28]=[CH:27]1)[CH3:20].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH2:19]([O:21][C:22](=[O:42])[C:23]([CH3:41])([CH3:40])[C:24](=[O:39])[CH:25]([O:31][C:32]1[CH:33]=[CH:34][C:35]([Cl:38])=[CH:36][CH:37]=1)[N:26]1[CH:30]=[CH:29][N:28]=[CH:27]1)[CH3:20]

Participants

4

Reactant 2

HCID 516892Sodium BicarbonateHCID 86738385HCID 86738385, compound

Product 1

HCID 54350404HCID 54350404, compoundYield 98%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

B 122.5 g (0.248 mol) of 4-(4-chlorophenoxy)-2,2-dimethyl-4-(imidazol-1-yl)-3-keto-butanoic acid ethyl ester 1,5-naphthalenedisulphonate (see Example 2) were suspended in 500 ml of methylene chloride and the suspension was stirred with 1,000 ml of saturated sodium bicarbonate solution for 0.5 hour. The organic phase was separated off, dried over sodium sulphate and concentrated. The residue crystallized on heating with 200 ml of petroleum ether. 85 g (98% of theory) of 4-(4-chlorophenoxy)-2,2-dimethyl-4-(imidazol-1-yl)-3-keto-butanoic acid ethyl ester of melting point 88° C. were obtained.

Workup

  1. customThe organic phase was separated off
  2. dry with materialdried over sodium sulphate
  3. concentrationconcentrated
  4. customThe residue crystallized
  5. temperatureon heating with 200 ml of petroleum ether

Sources & evidence

ORD record
ord-338c3e2a26984798a341a437e9a49609
Source dataset
uspto-grants-1982_05
Patent number
US04331674

Reaction notes

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