Acetic Anhydride → HCID 53922423, compound

HRID 128525Notes

Reaction equation

HRID 128525 reaction equation
[Cl:1][C:2]1[C:15]([F:16])=[C:14]([F:17])[C:13]([Cl:18])=[C:12]([F:19])[C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].[CH:20](OCC)(OCC)[O:21][CH2:22][CH3:23].C(OC(=O)C)(=O)C>>[Cl:1][C:2]1[C:15]([F:16])=[C:14]([F:17])[C:13]([Cl:18])=[C:12]([F:19])[C:3]=1[C:4]([C:6](=[CH:20][O:21][CH2:22][CH3:23])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]

Participants

4

Reactant 3

HCID 7918Acetic AnhydrideHCID 31214Ethyl orthoformateHCID 54482311HCID 54482311, compound

Product 1

HCID 53922423HCID 53922423, compound

Conditions

Temperature
150 °C

Procedure

A mixture of 31.5 g (0.1 mol) of ethyl (2,5-dichloro-3,4,6-trifluorobenzoyl)-acetate, 22.2 g (0.15 mol) of triethyl orthoformate and 25.5 g (0.25 mol) of acetic anhydride is heated under reflux for 2 hours (heating bath temperature of 150° C.). Low-boiling constituents are distilled off first under a waterpump vacuum and then under a high vacuum up to a bottom temperature of 130° C. The residue is used further as crude product.

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 2 hours
  3. distillationLow-boiling constituents are distilled off first under a waterpump vacuum
  4. customup to a bottom temperature of 130° C

Sources & evidence

ORD record
ord-bab83eb5dbfe4d5ba10795c671aa3dc4
Source dataset
uspto-grants-1995_11
Patent number
US05464796

Reaction notes

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