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ChemicalBook CAS DataBase List 2-FLUOROBUTANE
359-01-3

2-FLUOROBUTANE synthesis

8synthesis methods
-

Yield:359-01-3 71.2%

Reaction Conditions:

with methyl fluorosulfonate;1,8-diazabicyclo[5.4.0]undec-7-ene at 60 - 100;Inert atmosphere;Reagent/catalyst;Concentration;Temperature;

Steps:

1 Example 1

In a 300 ml volume glass reactor equipped with a stirring bar, a dropping funnel, a thermometer and a collection receiver, 56.7 g of 2-butanol and 85.3 g of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) were placed; then the contents were placed in a nitrogen atmosphere, and then the reactor was heated to 60° C.
When the internal temperature became constant, 50 g of the methanesulfonyl fluoride obtained in Production Example 1 was added dropwise to the reactor from the dropping funnel over approximately 1 hour.droppingAfter the completion of the dropwise addition, the reaction was continued at 60° C. for thrther 5 hours, and then the reactor was increased in temperature to 100° C., and the reaction was continued for further 1 hout Meanwhile, the distilled organic component was collected in a receiver immersed in a dry ice-ethanol bath. The organic substance collected in the receiver was analyzed with gas chromatography, and 27.6 g of 2-fluorobutane, the target product, was found to be obtained (yield with reference to methanesulfonyl fluoride: 71.2%).The structure of the target product was identified on the basis of the ‘H-NMR spectrum and the ‘9F-NMR spectrum.‘H-NMR (CDC13, TMS, ? ppm): 0.88 (t, 3H), 1.17(dq, 3H), 1.73 (m, 2H), 4.35 (m, 1H).‘9F-NMR (CDC13, CFC13, ? ppm): -173 (m, F)

References:

US2018/118642,2018,A1 Location in patent:Paragraph 0180-0184; 0193; 0194; 0204; 0205

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