Methanesulfonic Acid → HCID 23149398, compound

HRID 2074057Notes

Reaction equation

[F:1][C:2]([F:21])([S:17]([O-:20])(=[O:19])=[O:18])[CH:3]([O:8][C:9](=[O:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:4]([F:7])([F:6])[F:5].C([O:26][C:27]1[CH:32]=[CH:31][C:30]([S+:33]([C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)[C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)=[CH:29][CH:28]=1)(C)(C)C.CS(O)(=O)=O>ClCCl>[F:21][C:2]([F:1])([S:17]([O-:20])(=[O:18])=[O:19])[CH:3]([O:8][C:9](=[O:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:4]([F:5])([F:7])[F:6].[OH:26][C:27]1[CH:32]=[CH:31][C:30]([S+:33]([C:40]2[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=2)[C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)=[CH:29][CH:28]=1

Participants

Conditions

Temperature: 40 °C

Procedure

In 60 g of dichloromethane was dissolved 6.7 g of 4-tert-butoxyphenyldiphenylsulfonium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate (PAG4) prepared in Synthesis Example 14. Methanesulfonic acid, 0.1 g, was added to the solution, which was heated and stirred at 40° C. for 3 hours. The organic layer was washed with 30 g of water three times, and concentrated. Diethyl ether was added to the concentrate for crystallization. The crystals were filtered and dried, obtaining the target compound in an amount of 4.9 g.

Workup

customprepared in Synthesis Example 14
temperaturewas heated
washThe organic layer was washed with 30 g of water three times
concentrationconcentrated
additionDiethyl ether was added to the
concentrationconcentrate for crystallization
filtrationThe crystals were filtered
customdried
customobtaining the target compound in an amount of 4.9 g

Sources & evidence

ORD record: ord-e10bcd3a857e41448b4796a72dc2cde4
Source dataset: uspto-grants-2011_04
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07919226B2

Reaction notes

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