Zincchloride → HCID 178421619, compound

HRID 1585835Notes

Reaction equation

HRID 1585835 reaction equation
[C:1]12([Li])[CH2:10][CH:7]([CH2:8][CH2:9]1)[C:5](=[CH2:6])[C:2]2([CH3:4])[CH3:3].[Cl-].[Zn+2:13].[Cl-]>CCCCC.C(OCC)C>[C:1]12([Zn:13][C:1]34[CH2:10][CH:7]([CH2:8][CH2:9]3)[C:5](=[CH2:6])[C:2]4([CH3:4])[CH3:3])[CH2:10][CH:7]([CH2:8][CH2:9]1)[C:5](=[CH2:6])[C:2]2([CH3:4])[CH3:3]

Participants

5

Reactant 2

HCID 3007855ZincchlorideHCID 178506632HCID 178506632, compound

Product 1

HCID 178421619HCID 178421619, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 8003PentaneSolvent

Conditions

Temperature
-78 °C

Procedure

Thiele et al. Anorg. Allg. Chem. Chem. 1988, 561, 73. To a stirred suspension of 18.4 g 1-camphenyllithium in 250 mL n-pentane is added dropwise a solution of 9 g zincchloride in 300 mL diethylether at room temperature (keep the speed of addition in such a way that the solution is boiling smoothly). This reaction mixture is stirred for 3 h and is subsequently allowed to stand overnight. The precipitated LiCl is filtered off and the solvent of the filtrate is completely removed. The residue is solved in n-pentane and remaining LiCl is separated. The solution is the cooled to -78° C. The precipitated crystalls are filtered at low temperature and dried in vacuo. Yield: 12.5 g (60%).

Workup

  1. additionthe speed of addition in such a way that the solution
  2. waitto stand overnight
  3. filtrationThe precipitated LiCl is filtered off
  4. customthe solvent of the filtrate is completely removed
  5. customis separated
  6. filtrationThe precipitated crystalls are filtered at low temperature
  7. customdried in vacuo

Sources & evidence

ORD record
ord-2430a8cf027847499c3551dddf442871
Source dataset
uspto-grants-1999_08
Patent number
US05939568

Reaction notes

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