Methyl Acetate → HCID 22909616, compound

HRID 266708Notes

Reaction equation

HRID 266708 reaction equation
[NH2:1][C:2]1[NH:7][C:6]([CH3:8])=[C:5]([C:9]([O:11][CH3:12])=[O:10])[CH:4]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=2[Cl:20])[C:3]=1[C:21]#[N:22].[C:23](OC(=O)C)(=[O:25])[CH3:24].C(OC)(=O)C>CO>[C:23]([NH:1][C:2]1[NH:7][C:6]([CH3:8])=[C:5]([C:9]([O:11][CH3:12])=[O:10])[CH:4]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=2[Cl:20])[C:3]=1[C:21]#[N:22])(=[O:25])[CH3:24]

Participants

5

Reactant 3

HCID 6584Methyl AcetateHCID 7918Acetic Anhydride2×HCID 22909619HCID 22909619, compound

Product 1

HCID 22909616HCID 22909616, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

6.7 g (20 mmol) of methyl 6-amino-5-cyano-4-(2,3-dichlorophenyl)-2-methyl-1,4-dihydropyridine-3-carboxylate and 33.5 ml (350 mmol) of acetic anhydride are heated under reflux for 30 minutes. Excess acetic anhydride is then converted into methyl acetate by addition of methanol at 25° C., while stirring. The reaction solution is evaporated in vacuo and toluene is then shipped off from the residue twice in vacuo. The residue is then boiled up with 50 ml of toluene. The crystals which have separated out are filtered off and washed with toluene.

Workup

  1. temperatureunder reflux for 30 minutes
  2. customThe reaction solution is evaporated in vacuo and toluene
  3. customThe crystals which have separated out
  4. filtrationare filtered off
  5. washwashed with toluene

Sources & evidence

ORD record
ord-eb3f9b3a2b904f89aba96eeb48616e08
Source dataset
uspto-grants-1997_07
Patent number
US05652251

Reaction notes

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