Ammonium Acetate → HCID 14745920, compound

HRID 2372936Notes

Reaction equation

HRID 2372936 reaction equation
[Cl:1]/[C:2](/[C:9]([O:11][CH3:12])=[O:10])=[C:3](\Cl)/[C:4]([O:6][CH3:7])=[O:5].C([O-])(=O)C.[NH4+:17]>CN(C)C=O>[NH2:17]/[C:3](/[C:4]([O:6][CH3:7])=[O:5])=[C:2](\[Cl:1])/[C:9]([O:11][CH3:12])=[O:10]

Participants

4

Reactant 2

HCID 517165Ammonium AcetateHCID 3034513Dimethyl 2,3-dichloromaleate

Product 1

HCID 14745920HCID 14745920, compoundYield 83%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
120 °C

Procedure

53.25 g (0.25 mol) of dimethyl dichloromaleate were dissolved in 100 ml of dimethylformamide, and 48.16 g (0.625 mol) of ammonium acetate were added. The mixture was rapidly heated to 120° C. and stirred at 110° C. to 120° C. for one hour. The solvent was subsequently removed by distillation, the residue was taken up in methylene chloride, and the solution was washed with water. The methylene chloride was removed by distillation on an evaporator, and, after, recrystallization 40 g (83% yield) of dimethyl aminochloromaleate were obtained in the form of yellowish, cubic crystals (m.p. 96°-98° C.)

Workup

  1. customThe solvent was subsequently removed by distillation
  2. washthe solution was washed with water
  3. customThe methylene chloride was removed by distillation on an evaporator

Sources & evidence

ORD record
ord-368f3c8f27674e228fab78f363390abb
Source dataset
uspto-grants-1992_03
Patent number
US05101067

Reaction notes

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