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) 39.4 Parts of sodium difluorosulfoacetate (purity: 63.5%), 21.0 parts of 1-adamantanemethanol and 200 parts of dichloroethane were charged in a vessel, 24.0 parts of p-toluenesulfonic acid was added thereto, and the mixture was refluxed for 7 hours. After concentrating the mixture to eliminate dichloroethane, 250 parts of tert butyl methyl ether was added thereto, and the added mixture was stirred. The stirred mixture was filtered to obtain solid. 250 parts of acetonitrile was added to the solid. The mixture was stirred and filtrated. The filtrate was concentrated to obtain 32.8 parts of sodium salt of 1-adamantylmethyl difluorosulfoacetate.

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

ORD record

ord-2e5edd74053e45b99b8c3f05809a4118

Source dataset

uspto-grants-2012_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08124803B2