Reaktion #56154

Reaktionsgleichung

toluene

2-thenylamine

triethylamine

1,3-bis-chloromethyl-1,1,3,3-tetramethyl-disiloxane

→

4-(2-thienylmethyl)-2,2,6,6-tetra-methyl-1-oxa-4-aza-2,6-disilacyclohexane

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONTo a solution containing 22.6 g
2. 2
   Trocknenof acetonitrile dried over molecular sieves there
3. 3
   workup.ADDITIONis added 46.2 g
4. 4
   TemperaturAfter cooling the mixture
5. 5
   Waschenthe organic phase is then washed with two more portions of water
6. 6
   Einengenconcentrated
7. 7
   Sonstigeto give 61.5 g
8. 8
   workup.DISTILLATIONVacuum distillation through a Vigreux column

Vorschrift

To a solution containing 22.6 g. (0.2 mole) of 2-thenylamine, 44.4 g. (0.44 mole) of triethylamine and 50.0 g. of acetonitrile dried over molecular sieves there is added 46.2 g. (0.2 mole) of 1,3-bis-chloromethyl-1,1,3,3-tetramethyl-disiloxane. The resulting homogenized solution is allowed to stand for 3 days and then heated in a bath at 90° C. for 36 hours. After cooling the mixture is then equiliberated between toluene and water, the organic phase is then washed with two more portions of water and concentrated to give 61.5 g. of a crude oil. Vacuum distillation through a Vigreux column gives 4-(2-thienylmethyl)-2,2,6,6-tetra-methyl-1-oxa-4-aza-2,6-disilacyclohexane; b.p. 78° to 80° C. at 0.1 to 0.11 mm.

Quelle