Diphenyl Ether → HCID 178421951, compound

HRID 2304873Notes

Reaction equation

HRID 2304873 reaction equation
C(O[C:4]([C:6]1[C:10]([CH3:11])=[C:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[S:8][C:7]=1[NH:18][CH:19]=[CH:20][C:21](=[O:25])[CH:22]([CH3:24])[CH3:23])=[O:5])C.C1(OC2C=CC=CC=2)C=CC=CC=1>C(O)C>[OH:5][C:4]1[C:20]([C:21](=[O:25])[CH:22]([CH3:23])[CH3:24])=[CH:19][N:18]=[C:7]2[S:8][C:9]([C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)=[C:10]([CH3:11])[C:6]=12

Participants

4

Reactant 2

HCID 7583Diphenyl EtherHCID 701173894-Methyl-2-[(4-methyl-3-oxo-1-penten-1-yl)amino]-5-phenylthiophene-3-carboxylic acid ethyl ester

Product 1

HCID 178421951HCID 178421951, compoundYield 80.6%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

The compound obtained in Example 13 (50 g) and diphenylether (500 ml) were mixed and the ethanol formed as the reaction proceeded was distilled off while continuing the heating under reflux for 4 hours. After allowing to cool followed by distilling diphenylether off under reduced pressure a crude crystal was precipitated and washed with n-hexane to obtain the title compound (35.1 g, 80.6%).

Workup

  1. distillationproceeded was distilled off
  2. temperatureunder reflux for 4 hours
  3. temperatureto cool
  4. distillationby distilling diphenylether off under reduced pressure a crude crystal
  5. customwas precipitated
  6. washwashed with n-hexane

Sources & evidence

ORD record
ord-55a1f9b92ecb430ca1bb31c79ea9cf1b
Source dataset
uspto-grants-2002_08
Patent number
US06437132B2

Reaction notes

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