Tris(hydroxymethyl)aminomethane → Lithium Chloride

Participants

Reaction Steps

Tris[bis(trimethylsilyl)methyl chromium(III) was synthesized according to the method described in J. Chem. Soc. Dalton, 734 (1977) as follows. 0.48 g (3.03 mmol) of anhydrous chromium trichloride (a product of Nakalai Tesque Inc.) was put into a 100 ml flask the inner atmosphere of which had previously been replaced by nitrogen gas, and 50 ml of diethyl ether was then added to the flask to prepare a slurry. After cooling the flask with a dry ice-alcohol bath, 17. 1 ml (9.09 mmol) of a diethyl ether solution of bis(trimethylsilyl)methyl lithium synthesized in (1) above was added dropwise to the flask over 1 hour. After completion of the dropwise addition, temperature of the reaction solution was returned to room temperature and the solution was stirred for 2 hours. Precipitate of lithium chloride was formed. Solvent was completely removed under reduced pressure to obtain a dark green bulk. 80 ml of hexane was added to the bulk to dissolve the bulk therein, and after centrifugal separation, only a supernatant liquid was collected. Chromium concentration in the solution was measured and was found to be 0.0538 mol/liter, 2.80 g/liter.

Provenance & Evidence