Tributylamine → HCID 123897263, compound

HRID 1085982Notes

Reaction equation

HRID 1085982 reaction equation
C[SiH2][O:3][Si:4]([CH3:7])([CH3:6])C.[Cl:8][Si:9]([Cl:12])(Cl)Cl.C(N(CCCC)CCCC)CCC>C(Cl)Cl>[CH3:6][SiH:4]([CH3:7])[O:3][Si:9]([Cl:12])([Cl:8])[O:3][SiH:4]([CH3:6])[CH3:7].[CH3:6][SiH:4]([CH3:7])[O:3][Si:9]([Cl:12])([O:3][SiH:4]([CH3:6])[CH3:7])[O:3][SiH:4]([CH3:7])[CH3:6]

Participants

6

Reactant 3

HCID 7622TributylamineHCID 24816Silicon tetrachlorideHCID 57376941Tetramethyl disiloxane

Product 2

HCID 123897263HCID 123897263, compoundHCID 124024560HCID 124024560, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture containing 536 g (4.0 mol) of tetramethyldisiloxane, 170 g (1.0 mol) of tetrachlorosilane and 2 ml of a 25% solution of phosphonitrile chloride in methylene chloride is stirred at room temperature for 116 hours. About 1.1 ml of tri-n-butylamine are then added to deactivate the phosphonitrile chloride. The reaction mixture is stirred for 30 minutes and then subjected to fraction distillation. About 17 g of 1,1,5,5-tetramethyl-3,3-dichlorotrisiloxane are obtained at 30° to 43° C. and at 10 mbar, and 98 g of 1,1,5,5-tetra methyl-3-chloro-3-dimethylsiloxytrisiloxane are obtained at 44° to 47° C. and at 10 mbar, but the desired 1,1,5,5-tetramethyl-3,3-bis(dimethylsiloxy)trisiloxane is not obtained.

Workup

  1. stirringThe reaction mixture is stirred for 30 minutes
  2. distillationsubjected to fraction distillation

Sources & evidence

ORD record
ord-565a7a38bebf4be9b06686a821087fb4
Source dataset
uspto-grants-1991_04
Patent number
US05011962

Reaction notes

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