Acetic Anhydride → HCID 5244318, compound

HRID 1252284Notes

Reaction equation

HRID 1252284 reaction equation
[Cl:1][CH2:2][C:3](=[O:10])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH:11]([O-])([O-])[O:12][CH2:13][CH3:14].C(OC(=O)C)(=O)C>>[CH2:8]([O:7][C:5](=[O:6])[C:4](=[CH:11][O:12][CH2:13][CH3:14])[C:3]([CH2:2][Cl:1])=[O:10])[CH3:9]

Participants

4

Reactant 3

HCID 7918Acetic AnhydrideHCID 69484Ethyl 4-chloroacetoacetateHCID 53630039Ethylorthoformate

Product 1

HCID 5244318HCID 5244318, compoundYield 90.3%

Procedure

10 g (60.7 mM) of ethyl 4-chloroacetoacetate, 18 g (121 mM) of ethyl orthoformate and 25 g (245 mM) of acetic anhydride were stirred at 110° C. for 3 hours. Then, excessive ethyl orthoformate and acetic anhydride were distilled off under vacuum and the residue was recrystallized from hexane to obtain 12.1 g of a needle-like crystal with an yield of 90%.

Workup

  1. distillationThen, excessive ethyl orthoformate and acetic anhydride were distilled off under vacuum
  2. customthe residue was recrystallized from hexane

Sources & evidence

ORD record
ord-a8fb965cdfba455998b9b8025f062a16
Source dataset
uspto-grants-1988_05
Patent number
US04742165

Reaction notes

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