Boron trifluoride → HCID 70977307, compound

Participants

Reaction Steps

A solution of n-butyllithium (2.3 M in hexanes) is pumped (push-pull syringe-pump) to a ⅛″ tee with a pressure gauge and 2 feet of ⅛″ stainless steel tubing (for pre-cooling). This tubing is connected to a ¼ inch T-mixer. Thiazole (0.5 M in THF) is pumped using a pump, 100 μL head (Fluid Metering, Inc., Syosset, N.Y. USA) to 2 feet of ⅛″ stainless steel tubing (for pre-cooling) connected to the same T-mixer. The T-mixer is connected to a static mixer ¼-34 (5.3 mL) (Koflo Corporation, Cary, Ill. USA) connected to a ¼″ elbow and ¼″ stainless steel tubing of 6 inches in length (3.3 mL). This 6-inch length tubing is connected to another ¼″ T-mixer which is also connected to a feed of methyl 5-oxo-5,6,7,8-tetrahydronaphthalene-2-carboxylate and BF3 (0.5 M in THF, pumped with a FMI pump, 100 μL head), and to a second static mixer Koflo ¼-34 (5.3 mL) followed by a “loop” of ¼″ stainless steel (2.5 ft length, 16.8 mL). The reactor has a total volume of 30.7 mL, and is placed into a cold bath at −45° C. (±5° C., dry ice/acetone). The outlet stream is then connected to a ⅛″ T-mixer (outside of the cold bath) fed with methanol (FMI pump, 100 μL head) for in situ quenching, and is finally collected into an extractor containing MTBE and aqueous phosphoric acid (1.5 M). A flow diagram of the assembly is shown in FIG. 1.

Provenance & Evidence