Aethylzinntrichlorid [German] synthesis

4synthesis methods

Product Name:Aethylzinntrichlorid [German]
CAS Number:1066-57-5
Molecular formula:C2H5Cl3Sn
Molecular Weight:254.13

7646-78-8 Synthesis

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Yield:1066-57-5 76.7 %

Reaction Conditions:

at 115;Inert atmosphere;

Steps:

EtSnCl3 - Synthesis and Purification

Ph₃SnEt (637.8 g, 1.68 mol) was loaded into a 4-neck 2L roundbottom flask equipped with a magnetic stir bar, thermocouple, and nitrogen inlet adapter. In a nitrogen-fille glovebox, SnCl₄ (916g, 3.52 mol) was placed in a 500 mL addition funnel, which was then removed from the glovebox and attached to the 2L roundbottom flask. The apparatus was placed under N₂, and the SnCl₄ was added slowly over 8 hours directly to the solid Ph₃SnEt. The reaction mixture was heated to 115°C for 1 hour and then distilled using a jacketed 8" vigreaux distillation column at 1 torr between 67°C and 69°C. A 2-3 mL forecut was collected and the distillation was stopped when the head temperature reached 78°C. A second distillation was carried out using an 8" column packed with glass raschig rings at 1 torr with a head temperature of about 64°C to give EtSnCl₃ as a colorless liquid (327.16g, 108 mol, 76.7% yield) in >99.0% purity. ¹H-NMR (400 MHz, C₆D₆, 298K): 1.43 (t, 3H); 2.27 (q, 2H) ppm; ¹¹⁹Sn NMR (149 MHz, 298K): 2.03 ppm.