Diphenyl Ether → HCID 178469293, compound

HRID 66133Notes

Reaction equation

HRID 66133 reaction equation
[CH2:1]([O:3][C:4](=[O:22])[C:5]([NH:12][C:13]1[CH:19]=[CH:18][C:17](=[O:20])[C:16]([OH:21])=[CH:15][CH:14]=1)=[CH:6][C:7]([O:9]CC)=O)[CH3:2].C1(OC2C=CC=CC=2)C=CC=CC=1>CCCCCC>[CH2:1]([O:3][C:4]([C:5]1[NH:12][C:13]2[CH:14]=[CH:15][C:16](=[O:21])[C:17]([OH:20])=[CH:18][C:19]=2[C:7](=[O:9])[CH:6]=1)=[O:22])[CH3:2]

Participants

4

Reactant 2

HCID 7583Diphenyl EtherHCID 867362102-(4-Hydroxy-5-oxo-1,3,6-cycloheptatrien-1-ylamino)-2-butenedioic Acid Diethyl Ester

Product 1

HCID 178469293HCID 178469293, compound

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

2-(4-Hydroxy-5-oxo-1,3,6-cycloheptatrien-1-ylamino)-2-butenedioic acid diethyl ester (100 g, described in Example 1) is added in portions over 5 minutes to diphenyl ether (1000 ml) at reflux temperature. The solution is refluxed for 25 minutes and cooled to room temperature. Hexane (2000 ml) is added and the crystalline precipitate is collected. The precipitate is crystallized from acetic acid to obtain crystals of the title compound, mp > 300° C. and ν max 3270, 3170, 3100, 1740, 1620 and 1575 cm-1.

Workup

  1. temperatureat reflux temperature
  2. temperatureThe solution is refluxed for 25 minutes
  3. customthe crystalline precipitate is collected
  4. customThe precipitate is crystallized from acetic acid

Sources & evidence

ORD record
ord-f8e4898bb7ab44b88555d9c47a369ef8
Source dataset
uspto-grants-1978_12
Patent number
US04130649

Reaction notes

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