Hydrochloric Acid → HCID 11515081, compound

HRID 1270606Notes

Reaction equation

C([Li])CCC.[F:6][C:7]([F:15])([F:14])[CH:8]([OH:13])[C:9]([F:12])(F)[F:10].[C:16]([O:21][CH2:22][C:23](=[O:25])[CH3:24])(=[O:20])[C:17]([CH3:19])=[CH2:18].Cl.[O:27]1CCCC1>CCCCCC>[C:16]([O:21][CH2:22][C:23]([CH3:24])([OH:25])[C:9]([F:12])([F:10])[C:8]([OH:27])([OH:13])[C:7]([F:15])([F:14])[F:6])(=[O:20])[C:17]([CH3:19])=[CH2:18]

Participants

Conditions

Temperature: 5 °C

Procedure

Under nitrogen atmosphere and at 5° C., 129 ml of 1.6M n-butyllithium in hexane was added to a mixture of 16.8 g of 1,1,1,3,3,3-hexafluoro-2-propanol and 120 g of tetrahydrofuran, which was stirred for one hour at 5° C. Next, 14.2 g of 2-oxopropyl methacrylate was added at 5° C. The mixture was stirred for 10 hours, after which dilute hydrochloric acid was added to stop the reaction and neutralize the reaction mixture. Through conventional aqueous work-up and purification by silica gel column chromatography, 25.3 g of the target compound was obtained (yield 82%).

Workup

stirringThe mixture was stirred for 10 hours
customthe reaction
customThrough conventional aqueous work-up and purification by silica gel column chromatography

Sources & evidence

ORD record: ord-2aa5cbab80c548f0966fa19f04514e3e
Source dataset: uspto-grants-2007_04
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07202318B2

Reaction notes

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