HCID 86743973, compound → HCID 86743972, compound

HRID 1651586Notes

Reaction equation

HRID 1651586 reaction equation
C([C:3]1[C:4]([F:27])=[C:5]([C:19](=[O:26])[CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH:6]=[C:7]([F:18])[C:8]=1[CH:9]1[CH2:17][CH2:16][C:11]2([O:15][CH2:14][CH2:13][O:12]2)[CH2:10]1)C>C(OC(=O)C)(=O)C>[O:15]1[C:11]2([CH2:16][CH2:17][CH:9]([C:8]3[C:7]([F:18])=[CH:6][C:5]([C:19](=[O:26])[C:20](=[CH:13][O:12][CH2:11][CH3:10])[C:21]([O:23][CH2:24][CH3:25])=[O:22])=[C:4]([F:27])[CH:3]=3)[CH2:10]2)[O:12][CH2:13][CH2:14]1

Participants

3

Reactant 1

HCID 86743973HCID 86743973, compound

Product 1

HCID 86743972HCID 86743972, compound

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Procedure

A solution of 35.4 g (0.1 mol) of ethyl 2,5-difluoro-4-(1,4-dioxaspiro[4.4]non-7-yl)-β-oxobenzenepropanoic acid, ethyl ester 22.2 g (0.15 mol) triethyl orthoformate and 150 ml of acetic anhydride was heated at reflux for 4 hours. The solvent was removed in vacuo and the residue was triturated with ethanol and toluene (150 ml ea) which was also removed in vacuo, then high vacuo at 50°. The residue was used without further purification.

Workup

  1. temperatureat reflux for 4 hours
  2. customThe solvent was removed in vacuo
  3. customthe residue was triturated with ethanol and toluene (150 ml ea) which
  4. customwas also removed in vacuo
  5. customat 50°
  6. customThe residue was used without further purification

Sources & evidence

ORD record
ord-78f067db38734c2eb7448b42f9d49ae3
Source dataset
uspto-grants-1990_05
Patent number
US04929613

Reaction notes

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