Methanesulfonic Acid → HCID 85774566, compound

HRID 1287779Notes

Reaction equation

HRID 1287779 reaction equation
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([S:18](=[O:21])(=[O:20])[NH2:19])[C:10]=1[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:5]([OH:7])=[O:6].Br[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].CS(O)(=O)=O>C(O)CCCCC>[CH2:23]([O:6][C:5](=[O:7])[C:4]1[CH:8]=[C:9]([S:18](=[O:21])(=[O:20])[NH2:19])[C:10]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:2]([NH:1][CH2:4][CH2:3][CH2:2][CH2:10][CH2:9][CH3:8])[CH:3]=1)[CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]

Participants

5

Reactant 3

HCID 6395Methanesulfonic AcidHCID 81011-BromohexaneHCID 1199273-Amino-4-phenoxy-5-sulfamoylbenzoic acid

Product 1

HCID 85774566HCID 85774566, compound

Reagents, catalysts & solvents 1

HCID 81031-HexanolSolvent

Procedure

A mixture of 3-amino-4-phenoxy-5-sulphamyl-benzoic acid (4.62 g), 1-bromo-n-hexane (5 g), methanesulphonic acid (0.05 ml), and n-hexanol (40 ml) was refluxed for 60 hours. After cooling, the precipitated n-hexyl-3-n-hexylamino-4-phenoxy-5-sulphamyl-benzoate was collected and recrystallized from hexanol. The melting point was 137°-138° C.

Workup

  1. temperaturewas refluxed for 60 hours
  2. temperatureAfter cooling
  3. customthe precipitated n-hexyl-3-n-hexylamino-4-phenoxy-5-sulphamyl-benzoate was collected
  4. customrecrystallized from hexanol

Sources & evidence

ORD record
ord-18e2ccc5fc4b4b69b3ea0ef6d6badb96
Source dataset
uspto-grants-1976_10
Patent number
US03985777

Reaction notes

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