Triethylamine → HCID 131720044, compound

Participants

Reaction Steps

In a manner similar to that described above, 3-bromo-2,2-bis-(heptafluorobutoxymethyl)-1-propanol (250.0 g, 0.44 mole) was reacted with methanesulfonyl chloride (58.45 g, 0.51 mole) and triethylamine (52.62 g, 0.52 mole) in methylene chloride (400+200 ml). Additional methanesulfonyl chloride (2.96 g, 0.03 mole) was added to bring the reaction to completion. Washing and removal of the solvent gave 268.4 g (95.2%) of 3-bromo-2,2-bis(heptafluorobutoxymethyl)-1-propanol mesylate (4), a yellow oil: IR 2940, 1350, 1223, 1176, and 1120 cm-1 ; 1H NMR (CDCl3) 3.02 (s, 3H), 3.49 (s, 2H), 3.68 (s, 4H), 3.97 (t, J=13.3 Hz, 4H), and 4.24 (s, 2H); 13C NMR (CDCl3) 31.66, 36.64, 44.60, 67.81 (t, J=26.44), 68.36, and 70.30. Anal. Calcd for C14H15BrF14O5S: C, 26.22; H, 2.36; Br, 12.46, F, 41.48. Found: C, 25.95; H, 2.33; Br, 12.88.

Provenance & Evidence