Hydrochloric Acid → Sodium difluorosulfoacetate

Temperature

100 °C

230 Parts of 30% aqueous sodium hydroxide solution was added into a mixture of 100 parts of methyl difluoro(fluorosulfonyl)acetate and 250 parts of ion-exchanged water in a ice bath. The added mixture was heated and refluxed at 100° C. for 3 hours. After cooling, the cooled mixture was neutralized with 88 parts of conc. hydrochloric acid and concentrated to obtain 164.8 parts of sodium difluorosulfoacetate (containing inorganic salt, purity: 62.6%). (2) 5.0 Parts of sodium difluorosulfoacetate (purity: 62.8%), 2.6 parts of 4-oxo-1-adamantanol and 100 parts of ethylbenzene were charged in a vessel, 0.8 parts of conc. sulfuric acid was added thereto, and the mixture was refluxed for 42 hours. After cooling, the resultant mixture was filtrated to obtain crystals, and the crystals were washed with tert-butyl methyl ether to obtain 5.5 parts of sodium salt of 4-oxo-1-adamantyl difluorosulfoacetate. The purity thereof was 35.6%, which was determined by 1H-NMR.

1. temperatureThe added mixture was heated
2. temperatureAfter cooling
3. concentrationconcentrated

ORD record

ord-750f3b4800fa4fa5a7c97fa3f7e30eea

Source dataset

uspto-grants-2012_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08124803B2