Water → HCID 57526215, compound

Temperature

150 °C

A mixture of CF3OCF2CF2CH2CH2I, (92 g, 0.27 mol) and N-methyl-formamide (119 mL), was heated to 150° C. for 26 hours. Then the reaction was cooled to 100° C., followed by the addition of water to separate the crude ester. Ethyl alcohol (30 mL) and p-toluene sulfonic acid (1.03 g) were added to the crude ester, and the reaction was stirred at 70° C. for 15 minutes. Then ethyl formate and ethyl alcohol were distilled out to give a crude product. The crude product was dissolved in ether, washed with aqueous sodium sulfite, water, and brine in turn, then dried over magnesium sulfate. The product was then distilled to give 44 g of CF3OCF2CF2CH2CH2OH in 71% yield.

1. temperatureThen the reaction was cooled to 100° C.
2. customto separate the crude ester
3. additionEthyl alcohol (30 mL) and p-toluene sulfonic acid (1.03 g) were added to the crude ester
4. distillationThen ethyl formate and ethyl alcohol were distilled out
5. customto give a crude product
6. washwashed with aqueous sodium sulfite, water, and brine in turn
7. dry with materialdried over magnesium sulfate
8. distillationThe product was then distilled

ORD record

ord-ad2bf96bb0784d4ba8a8501dc247077e

Source dataset

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07815816B2