Bromide ion → 4-Heptanol, 1,1,1,7,7,7-hexafluoro-

3-Bromo-1,1,1-trifluoropropane (31 g, 0.175 mol) was dissolved in THF (175 mL). Mg (4.2 g, 0.175 mol) was placed in a 1 L, 3-necked round-bottom flask equipped with a condenser, nitrogen inlet and thermometer. The bromide solution (10 mL) was added to cover the magnesium and upon stirring a mild exotherm commenced. The temperature was kept <40° C. by immersing the flask in a bowl of water. The bromide was added slowly to maintain this mild exothermic reaction. When the exotherm had subsided the mixture was cooled in ice-water and methyl formate (7 mL, 0.11 mol) in THF (175 mL) was added. The mixture was stirred for 30 min and then quenched with NH4Cl (aq.soln. 100 mL). The mixture was extracted with ethyl acetate. The organic extracts were washed with brine, dried (MgSO4) and evaporated.

1. customequipped with a condenser, nitrogen inlet
2. customwas kept <40° C.
3. temperatureto maintain
4. customthis mild exothermic reaction
5. stirringThe mixture was stirred for 30 min
6. customquenched with NH4Cl (aq.soln. 100 mL)
7. extractionThe mixture was extracted with ethyl acetate
8. washThe organic extracts were washed with brine
9. dry with materialdried (MgSO4)
10. customevaporated

ORDレコード

ord-4fd8e24202324ca78ff02b232c2c713f

出典データセット

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08389547B2