Hydrochloric Acid → HCID 11305015, compound

HRID 915619Notes

Reaction equation

HRID 915619 reaction equation
ClC([O:4][CH2:5][CH3:6])=O.[F:7][C:8]1[CH:13]=[C:12]([F:14])[CH:11]=[CH:10][C:9]=1[C:15]1[CH:23]=[C:19]([C:20]([OH:22])=[O:21])[C:18]([OH:24])=[C:17]([I:25])[CH:16]=1.[CH3:26]N(C)C1C=CC=CC=1.Cl>C1C=CC=CC=1>[F:7][C:8]1[CH:13]=[C:12]([F:14])[CH:11]=[CH:10][C:9]=1[C:15]1[CH:16]=[C:17]([I:25])[C:18]([O:24][C:5]([CH2:6][CH3:26])=[O:4])=[C:19]([C:20]([OH:22])=[O:21])[CH:23]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 949N,N-DimethylanilineHCID 10928Ethyl chloroformateHCID 43695632',4'-Difluoro-4-hydroxy-5-iodo-1,1'-biphenyl-3-carboxylic acid

Product 1

HCID 11305015HCID 11305015, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

0.928 g (0.0086 mmol) of ethyl chloroformate was added to a mixture of 2.5 g (0.0061 mmol) of 5-(2,4-difluorophenyl)-3-iodo-salicylic acid in 6 ml of benzene and 1.728 g (0.014 mmol) of dimethylaniline. The mixture was stirred at room temperature for 3 hr. Ice and a solution of 2.5 N of HCl were added. It was extracted with dichloromethane and the organic phase was dried over magnesium sulphate. The solvent was evaporated at low pressure and the crude was recrystalized from a chloroform-hexane mixture.

Workup

  1. extractionIt was extracted with dichloromethane
  2. dry with materialthe organic phase was dried over magnesium sulphate
  3. customThe solvent was evaporated at low pressure
  4. customthe crude was recrystalized from a chloroform-hexane mixture

Sources & evidence

ORD record
ord-99f3574c8e4b4bb0bea27a7ab2c535f1
Source dataset
uspto-grants-2007_09
Patent number
US07265245B2

Reaction notes

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