Tris(hydroxymethyl)aminomethane → Lithium Chloride

HRID 1059047Notes

Reaction equation

HRID 1059047 reaction equation
C(O)C(N)(CO)CO.[Cl-:9].[Cl-].[Cl-].[Cr+3:12].[CH3:13][Si:14]([CH:17]([Li:22])[Si:18]([CH3:21])([CH3:20])[CH3:19])([CH3:16])[CH3:15]>C(OCC)C>[CH3:13][Si:14]([CH:17]([Cr+2:12])[Si:18]([CH3:21])([CH3:20])[CH3:19])([CH3:16])[CH3:15].[Cl-:9].[Li+:22]

Participants

6

Reactant 3

HCID 6503Tris(hydroxymethyl)aminomethaneHCID 6452300Chromium(3+) trichlorideHCID 178506911HCID 178506911, compound

Product 2

HCID 433294Lithium ChlorideHCID 178504295HCID 178504295, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

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trichloride (a product of Nakalai Tesque Inc.) was put into a 100 ml flask the inner atmosphere of which had previously been replaced by nitrogen gas, and 50 ml of diethyl ether was then added to the flask to prepare a slurry.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.

Workup

  1. custom) was put into a 100 ml flask
  2. additionwas then added to the flask
  3. customto prepare a slurry
  4. temperatureAfter cooling the flask with a dry ice-alcohol bath
  5. additionabove was added dropwise to the flask over 1 hour
  6. additionAfter completion of the dropwise addition, temperature of the reaction solution
  7. customwas returned to room temperature

Sources & evidence

ORD record
ord-11b4b5f49c0645c19bf21d0d67bc54f8
Source dataset
uspto-grants-2003_02
Patent number
US06518375B1

Reaction notes

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