Heptane → 2-Chloro-2,4,4,6,6,8,8-heptamethyl-1,3,5,7,2,4,6,8-tetroxatetrasilocane
Reaction equation
[CH3:1][SiH:2]1[O:9][Si:8]([CH3:11])([CH3:10])[O:7][Si:6]([CH3:13])([CH3:12])[O:5][Si:4]([CH3:15])([CH3:14])[O:3]1.CCCCCCC.[Cl:23]Cl>>[Cl:23][Si:2]1([CH3:1])[O:3][Si:4]([CH3:14])([CH3:15])[O:5][Si:6]([CH3:13])([CH3:12])[O:7][Si:8]([CH3:11])([CH3:10])[O:9]1Participants
Conditions
- Temperature
- 0 °C
Procedure
To a 1000 mL three-necked round bottom flask equipped with a magnetic stirring bar, a thermometer, an inlet for gases and an outlet fitted with a drying tube, was charged the following: 37.17 g (77.87 mmol) of heptamethylcyclotetrasiloxane (59.2% in octamethylcyclotetrasiloxane) and 521.9 g (5214 mmol) of heptane. The mixture was cooled in an ice bath to 0° C. Chlorine (Cl2) was bubbled through the stirred mixture at a rate such that the temperature did not rise above 10° C. The addition of the chlorine was continued until a persistent yellow color, accompanied by a drop in temperature, was observed. Nitrogen gas was bubbled through the solution to remove the HCl generated in the reaction and the excess Cl2. A yield of 100% under anhydrous conditions was determined by gas chromatographic analysis.
Workup
- customTo a 1000 mL three-necked round bottom flask equipped with a magnetic stirring bar
- customa thermometer, an inlet for gases and an outlet fitted with a drying tube
- customChlorine (Cl2) was bubbled through the stirred mixture at a rate such that the temperature
- customdid not rise above 10° C
- additionThe addition of the chlorine
- customNitrogen gas was bubbled through the solution
- customto remove the HCl
- customgenerated in the reaction
Sources & evidence
- ORD record
- ord-ef45a58c30ae41c687fb4af7dd18a75e
- Source dataset
- uspto-grants-1994_07
- Patent number
- US05330836
Reaction notes
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