Organic Lab Reactions 74


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DIRECT FLUORINATION AND ADDITION OF FLUORINE 69 is continued for another hour; then the mass is cooled with solid carbon dioxide and allowed to distil through water. The crude ethyl fluoride,' obtained in 81% yield, is passed through a soda-lime tube, then recti- fied, b.p. --37.7°. Isopropyl Fluoride. 46 The procedure is the same as for ethyl fluoride except that the temperature is kept at 0°, and the ratio of hydrogen fluoride to propylene is held to 1.08. The yield is 61%; isopropyl fluoride boils at -10.1°. Cyclohexyl Fluoride. 46 In a copper container fitted with inlet, outlet; and stirrer is placed 200 g. of anhydrous hydrogen fluoride. After cool- ing to —35°, 400 g. of precooled cyclohexene is added dropwise over a period of seventy-five minutes. The reaction mixture is poured into a copper beaker filled with cracked ice, stirred, decanted, dried, and dis- tilled under 300 mm. pressure (b.p. 71-71.4°). The yield is 60%; at 10° it is only 54%. 2,2-Difluoropropane
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