Ammonium Carbonate → HCID 178518413, compound

HRID 892339Notes

Reaction equation

HRID 892339 reaction equation
[F:1][C:2]([F:15])([F:14])[C:3]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([CH:12]=O)=[CH:11][C:5]=2[N:4]=1.[C:16](=[O:19])([O-])[O-].[NH4+:20].[NH4+:21].[Na].[CH2:23]([OH:25])C.O>>[F:1][C:2]([F:15])([F:14])[C:3]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([CH:12]3[NH:21][C:23](=[O:25])[NH:20][C:16]3=[O:19])=[CH:11][C:5]=2[N:4]=1

Participants

5

Reactant 4

HCID 517111Ammonium CarbonateHCID 5360545SodiumHCID 19096565Water ethanolHCID 178519338HCID 178519338, compound

Product 1

HCID 178518413HCID 178518413, compound

Procedure

29.2 g (0.136 mol) of 14d in ethanol/water are reacted with 55 g (0.573 mol) of ammonium carbonate and 10.4 g (0.212 mol) of sodium cynanide in analogy to Example 1c. After removal of ethanol by distillation, the solution is acidified with 2N HCl to pH 2 at 0° C., then the pH is returned to 4.5 and the solution is extracted several times with ethyl acetate. The combined ethyl acetate phases are washed with sodium chloride solution, dried and evaporated.

Workup

  1. customAfter removal of ethanol
  2. distillationby distillation
  3. customis acidified with 2N HCl to pH 2 at 0° C.
  4. extractionthe solution is extracted several times with ethyl acetate
  5. washThe combined ethyl acetate phases are washed with sodium chloride solution
  6. customdried
  7. customevaporated

Sources & evidence

ORD record
ord-5211490d564b4d208db7c19b45e17fde
Source dataset
uspto-grants-1992_06
Patent number
USRE033948

Reaction notes

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