碘滴定
Titration Using I2
A 10-mL round-bottom flask equipped with a magnetic stirring bar and a septum was heated with a heat gun under reduced pressure and cooled to r.t. under an argon atmosphere. The dry flask was charged with accurately weighed I2 (254 mg, 1 mmol), fitted with a rubber septum, and flushed with argon. The sat. solution of LiCl in THF (3–5 mL) was added and stirring was started. After the iodine was completely dissolved, the resulting brown solution was cooled to 0 °C in an ice bath and the organometallic reagent was added dropwise via a 1.00-mL syringe (0.01-mL graduations) until the brown color disappeared. The amount consumed contains 1 equiv of the organometallic reagent relative to iodine in the case of monoorganometallic reagents and 0.5 equiv for diorganometallic reagents.
摘自——Krasovskiy, A.; Knochel, P. Synthesis 2006, 890，
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碘滴定
Titration Using I2
A 10-mL round-bottom flask equipped with a magnetic stirring bar and a septum was heated with a heat gun under reduced pressure and cooled to r.t. under an argon atmosphere. The dry flask was charged with accurately weighed I2 (254 mg, 1 mmol), fitted with a rubber septum, and flushed with argon. The sat. solution of LiCl in THF (3–5 mL) was added and stirring was started. After the iodine was completely dissolved, the resulting brown solution was cooled to 0 °C in an ice bath and the organometallic reagent was added dropwise via a 1.00-mL syringe (0.01-mL graduations) until the brown color disappeared. The amount consumed contains 1 equiv of the organometallic reagent relative to iodine in the case of monoorganometallic reagents and 0.5 equiv for diorganometallic reagents.
摘自——Krasovskiy, A.; Knochel, P. Synthesis 2006, 890，