Potassium Carbonate → HCID 53840462, compound

HRID 1154834Notes

Reaction equation

HRID 1154834 reaction equation
C(=O)([O-])[O-].[K+].[K+].[CH3:7][O:8][N:9]=[C:10]([C:15]([O:20][CH2:21][CH3:22])([O:17][CH2:18][CH3:19])[CH3:16])[C:11]([O:13][CH3:14])=[O:12].S(Cl)([Cl:26])(=O)=O>C(Cl)(Cl)Cl>[CH3:7][O:8][N:9]=[C:10]([C:15]([O:20][CH2:21][CH3:22])([O:17][CH2:18][CH3:19])[CH2:16][Cl:26])[C:11]([O:13][CH3:14])=[O:12]

Participants

5

Procedure

Anhydrous potassium carbonate (8.89 g) was added to a solution of methyl 2-methoxyimino-3,3-diethoxybutyrate (syn isomer, 10 g) in chloroform (40 ml). Sulfuryl chloride (6.94 g) was added to the suspension at -6 to -2° C. over 50 minutes, and stirred at -5° to -2° C. for 10 minutes. After removing the solvent from the resultant mixture, ethanol (10 ml) was added to the residue and stirred for 30 minutes. Water (25 ml) was added to the mixture, and the mixture was extracted with diisopropyl ether (20 ml) twice. The extract was washed with water (10 ml) and a saturated aqueous solution of sodium chloride (5 ml) subsequently, and dried over magnesium sulfate. The solution was evaporated in vacuo to give methyl 2-methoxyimino-3,3-diethoxy-4-chlorobutyrate (syn isomer, 11.23 g).

Workup

  1. customAfter removing the solvent from the resultant mixture, ethanol (10 ml)
  2. additionwas added to the residue
  3. stirringstirred for 30 minutes
  4. additionWater (25 ml) was added to the mixture
  5. extractionthe mixture was extracted with diisopropyl ether (20 ml) twice
  6. washThe extract was washed with water (10 ml)
  7. dry with materiala saturated aqueous solution of sodium chloride (5 ml) subsequently, and dried over magnesium sulfate
  8. customThe solution was evaporated in vacuo

Sources & evidence

ORD record
ord-c15f79b3e30244558e6d475898d71a14
Source dataset
uspto-grants-1981_11
Patent number
US04298529

Reaction notes

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