Ammonium Acetate → HCID 21480574, compound

HRID 1490166Notes

Reaction equation

HRID 1490166 reaction equation
C([O:3][C:4](=O)[CH:5]([C:23]#[N:24])[CH2:6][CH:7]1[C:12](=O)[CH2:11][CH2:10][CH:9]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=2)[CH2:8]1)C.C([O-])(=O)C.[NH4+:30]>CO.O>[CH3:22][O:21][C:18]1[CH:19]=[CH:20][C:15]([CH2:14][CH:9]2[CH2:10][CH2:11][C:12]3[NH:30][C:4](=[O:3])[CH:5]([C:23]#[N:24])[CH2:6][C:7]=3[CH2:8]2)=[CH:16][CH:17]=1

Participants

5

Reactant 2

HCID 517165Ammonium AcetateHCID 57025170HCID 57025170, compound

Product 1

HCID 21480574HCID 21480574, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

2-Cyano-3-[3-(4-methoxyphenyl)methyl-6-oxocyclohexanyl]propanoic acid ethyl ester (1 g) (prepared as described in Example 5(a)) in methanol (10 ml) was treated with ammonium acetate (2.2 g) and left to stir at room temperature for 2 hours. The reaction mixture was diluted with water and a solid crystallised out. The solid was mixed with water and methanol, and the methanol removed under reduced pressure. The mixture was extracted into ethyl acetate, dried (MgSO4), and solvent evaporated to give the title compound as the quarterhydrate, mp 158°-9° C.

Workup

  1. waitleft
  2. customa solid crystallised out
  3. additionThe solid was mixed with water and methanol
  4. customthe methanol removed under reduced pressure
  5. extractionThe mixture was extracted into ethyl acetate
  6. dry with materialdried (MgSO4), and solvent
  7. customevaporated

Sources & evidence

ORD record
ord-f52851d9e290443a862867aeaa441b35
Source dataset
uspto-grants-1997_10
Patent number
US05681839

Reaction notes

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