Tributylamine → 3,3-Dichloro-1,1,1,5,5,5-hexamethyltrisiloxane
Reaction equation
C[Si](C)(C)[O:3][Si:4]([CH3:7])([CH3:6])[CH3:5].[Cl:10][Si:11]([Cl:14])(Cl)Cl.C(N(CCCC)CCCC)CCC>C(Cl)Cl>[Cl:10][Si:11]([Cl:14])([O:3][Si:4]([CH3:5])([CH3:6])[CH3:7])[O:3][Si:4]([CH3:7])([CH3:6])[CH3:5]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
About 1.9 ml of a 25% solution of phosphonitrile chloride in methylene chloride are added at room temperature with stirring to a mixture containing 486 g (3.0 mol) of hexamethyldisiloxane and 170 g (1.0 mol) of tetrachlorosilane. After the mixture has been stirred at room temperature for 8 hours, the catalyst is deactivated by adding 2.2 ml of tri-n-butylamine. Distillation of the reaction mixture at 18° to 34° C. and at 2 mbar gives 55 g of 3,3-dichlorohexamethyltrisiloxane, but no 3-chloro-3-trimethylsiloxyhexamethyltrisiloxane. Likewise the desired 3-chloro-3-trimethylsiloxyhexamethyltrisiloxane is neither found in the distillation residue (12 g) nor in the cold trap (583 g of a mixture of trimethylchlorosilane and 1,1,1-trichloro-3,3,3-trimethyldisiloxane).
Workup
- stirringAfter the mixture has been stirred at room temperature for 8 hours
- distillationDistillation of the reaction mixture at 18° to 34° C.
Sources & evidence
- ORD record
- ord-fa18798df8fc4111ad4369f087e0716d
- Source dataset
- uspto-grants-1991_04
- Patent number
- US05011962
Reaction notes
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