Dichloromethane → 1,2-Epoxydodecane

Under a flow of F2 (10% in N2) of 8.9 ml min−1 (1.49 mmol h−1) fed through conduit 12, MeCN:H2O (4:1, 5.50 ml) was added to conduit 16 at a rate of 5.50 ml −1 (60.4 mmol h−1). A solution of dodec-1-ene 24 (0.25 g, 1.49 mmol) (in a 1:1 mixture of DCM:MeCN) was added to pot reactor 22 prior to reaction. The HOF.MeCN thus generated was passed via conduit 20 into the pot reactor 22. Following reaction and purging with nitrogen, the reaction mixture was then transferred from pot reactor 22 to a vessel containing 100 ml of sodium bicarbonate solution, washed with DCM (3×75 ml), dried over MgSO4 and filtered. The solvent was removed under reduced pressure to yield 2-decyloxirane (0.233 g, 1.27 mmol, 85%) as a pale yellow oil, with no further purification required.

1. additionwas added
2. customto reaction
3. customreaction
4. custompurging with nitrogen
5. customthe reaction mixture was then transferred from pot reactor
6. addition22 to a vessel containing 100 ml of sodium bicarbonate solution
7. washwashed with DCM (3×75 ml)
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. customThe solvent was removed under reduced pressure

ORD record

ord-55a0a80c1f9a44489a74dfb4166e39cc

Source dataset

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08609873B2