Methanesulfonic Acid → HCID 86634874, compound

HRID 2366407Notes

Reaction equation

HRID 2366407 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[C:10](/[C:16](=[CH:19]/[C:20]2[S:21][C:22]([N:25]3[CH2:30][CH2:29][N:28]([CH2:31][CH2:32][OH:33])[CH2:27][CH2:26]3)=[CH:23][CH:24]=2)/[C:17]#[N:18])[CH:11]=[CH:12][C:13]=1[O:14][CH3:15]>C(O)C>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[C:10](/[C:16](=[CH:19]/[C:20]2[S:21][C:22]([N:25]3[CH2:30][CH2:29][N:28]([CH2:31][CH2:32][OH:33])[CH2:27][CH2:26]3)=[CH:23][CH:24]=2)/[C:17]#[N:18])[CH:11]=[CH:12][C:13]=1[O:14][CH3:15]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 11965334HCID 11965334, compound

Product 1

HCID 86634874HCID 86634874, compoundYield 85%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
70 °C

Procedure

Methanesulfonic acid (81.6 μL) and ethanol (10 mL) were added to Compound 9 (500 mg), and the mixture was heated for dissolution (external temperature: 70° C.). The solution was returned to room temperature, followed by stirring overnight. The precipitated crystals were recovered through filtration, and the recovered crystals were washed sequentially with a small amount of ethanol and hexane. The crystals were thoroughly dried, to thereby yield the target product (yield: 530 mg, 85%).

Workup

  1. customwas returned to room temperature
  2. filtrationThe precipitated crystals were recovered through filtration
  3. washthe recovered crystals were washed sequentially with a small amount of ethanol and hexane
  4. customThe crystals were thoroughly dried

Sources & evidence

ORD record
ord-c38a2ac709964596a1e5e2003457340e
Source dataset
uspto-grants-2014_04
Patent number
US08697742B2

Reaction notes

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