Methanesulfonic Acid → HCID 15718098, compound

HRID 982454Notes

Reaction equation

HRID 982454 reaction equation
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.CS(O)(=O)=O.[C:20]([C:23]1[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][C:24]=1[C:31]1[CH:36]=[CH:35][C:34]([C:37]([OH:39])=[O:38])=[CH:33][CH:32]=1)(O)=[O:21]>>[C:37]([C:34]1[CH:35]=[CH:36][C:31]2[C:24]3[C:23](=[CH:28][CH:27]=[C:26]([O:29][CH3:30])[CH:25]=3)[C:20](=[O:21])[C:32]=2[CH:33]=1)([OH:39])=[O:38]

Participants

4

Reactant 3

HCID 6395Methanesulfonic Acid2×HCID 14812Phosphorus oxide (P4O10)HCID 15718053HCID 15718053, compound

Product 1

HCID 15718098HCID 15718098, compoundYield 74.5%

Conditions

Temperature
40 °C

Procedure

A mixture of 2.5 g of phosphorous pentoxide and 25 ml of methanesulfonic acid were stirred together under a nitrogen atmosphere overnight. To this mixture were added 2.3 g of 2,4'-dicarboxy-5-methoxybiphenyl. The reaction mixture was stirred at room temperature for six hours with the addition of methanesulfonic acid to keep the mixture sufficient for stirring. The mixture was then warmed to 40° C. for one hour, cooled, and poured into ice water. The resulting yellow-green precipitate was recovered by filteration, washed with water, and dried to provide 1.6 g of the desired subtitle intermediate.

Workup

  1. stirringfor stirring
  2. temperaturecooled
  3. customThe resulting yellow-green precipitate was recovered by filteration
  4. washwashed with water
  5. customdried

Sources & evidence

ORD record
ord-12937401ac8a47e6b9e13cb6781525ff
Source dataset
uspto-grants-1991_02
Patent number
US04996230

Reaction notes

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