Disilane, 1,1,2-trichloro-1,2,2-trimethyl- → HCID 14008873, compound

HRID 986834Notes

Reaction equation

HRID 986834 reaction equation
[Cl:1][Si:2](Cl)([CH3:7])[Si:3]([Cl:6])([CH3:5])[CH3:4].[C:9]1([Li])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>>[Cl:1][Si:2]([CH3:7])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[Si:3]([Cl:6])([CH3:5])[CH3:4]

Participants

3

Reactant 2

HCID 83551Disilane, 1,1,2-trichloro-1,2,2-trimethyl-HCID 178506676HCID 178506676, compound

Product 1

HCID 14008873HCID 14008873, compound

Procedure

1,1,2-trichloro-1,2,2-trimethyl disilane 103.8 g (0.5 mole) and petroleum ether 200 g were placed in the same type of reaction apparatus as used in the above Comparative Example, and an petroleum ether solution of phenyl lithium 42.5 g (0.5 mole) was dropwise added thereto for 3 hours while stirring at the reaction temperature of 25° to 30° C. After the dropwise addition, the stirring was continued for 2 hours at 25° to 30° C. to complete the reaction. In order to identify the reaction product, the product obtained by separating the by-produced lithium salt by filtration was subjected to 1H-NMR spectrum (C6D6) analysis in the same manner as in the above Comparative Example. As this result, it was proved that 1,1-dichloro-1,2,2-trimethyl-2-phenyl disilane was not substantially produced and that 1,2-dichloro-1,2,2-trimethyl-1-phenyl disilane could be produced at a favourable selectivity. The reaction product was then purified by a normal purification method to obtain 1,2-dichloro-1,2,2-trimethyl-1-phenyldisilane 113.4 g at the yield of 91%.

Workup

  1. additionAfter the dropwise addition
  2. waitthe stirring was continued for 2 hours at 25° to 30° C.
  3. customthe reaction
  4. customthe product obtained
  5. customby separating the by-produced lithium salt
  6. filtrationby filtration
  7. customwas not substantially produced

Sources & evidence

ORD record
ord-10bbd979d7d640358ad739170ac59c2b
Source dataset
uspto-grants-1987_12
Patent number
US04716240

Reaction notes

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