Hexamethyldisilazane → HCID 178448203, compound

HRID 1261551Notes

Reaction equation

HRID 1261551 reaction equation
[CH2:1]([Mg:5]CC)[CH2:2][CH2:3][CH3:4].[CH3:8][Si:9]([CH3:16])([CH3:15])[NH:10][Si:11]([CH3:14])([CH3:13])[CH3:12]>CCCCCCC>[CH3:8][Si:9]([N-:10][Si:11]([CH3:14])([CH3:13])[CH3:12])([CH3:16])[CH3:15].[CH2:1]([Mg+:5])[CH2:2][CH2:3][CH3:4]

Participants

4

Reactant 2

HCID 13838HexamethyldisilazaneHCID 178448194HCID 178448194, compound

Product 1

HCID 178448203HCID 178448203, compound

Reagents, catalysts & solvents 1

HCID 8900HeptaneSolvent

Procedure

A Fischer-Porter test tube size aerosol compatibility vessel is fitted with a tee and valves to maintain a nitrogen atmosphere. A heptane solution of butyl ethyl magnesium (25 mL, 16 mMoles) and hexamethyl disilazane (3.3 mL) are injected by syringe into the tube. Gas is evolved when the two reactants are contacted. After 1 hour and 40 minutes at room temperature, the contents of the tube are transferred to a flask for solvent evaporation without exposing the contents to air. After about four hours at room temperature, with a N2 flow, crystals began to appear in the viscous residue. The following day, the residue appears to be completely solidified. A vacuum is applied for two hours to remove any volatiles.

Workup

  1. customA Fischer-Porter test tube size aerosol compatibility vessel is fitted with a tee and valves
  2. temperatureto maintain a nitrogen atmosphere
  3. custom40 minutes at room temperature, the contents of the tube are transferred to a flask for solvent evaporation
  4. waitAfter about four hours at room temperature
  5. waitA vacuum is applied for two hours
  6. customto remove any volatiles

Sources & evidence

ORD record
ord-3c946b0a8b3d45f8a030b81b94a4dfb4
Source dataset
uspto-grants-2013_06
Patent number
US08470939B2

Reaction notes

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