Yield:81177-90-4 75.98%

Reaction Conditions:

Stage #1: methoxyethenewith n-butyllithium;N,N,N,N,-tetramethylethylenediamine;potassium isopropoxide in tetrahydrofuran;hexane at -50 - -30; for 2 h;Inert atmosphere;Stille Carbonyl Synthesis;
Stage #2: tributyltin chloride in tetrahydrofuran;hexane;water at -78; for 10 h;

Steps:

3 Example 3: Preparation of tributyl (α-methoxyethyl) tin

Under the protection of nitrogen, the 84g potassium ethoxide (1 μM), 232g tetramethyl ethylene diamine (2 μM), added to the 1600 ml hexane, lowering the temperature to -40 °C; instillment mole concentration is 2.5 n-butyllithium in hexane solution of 500 ml, 2 hours after the completion of the dropping, the reaction at the temperature for 1 hour, then reducing to -50 °C; will be 104.4g vinyl methyl ether (1.8 μM) is dissolved in 300 ml anhydrous in tetrahydrofuran, drop into the entry into the above-mentioned mixed solution, keep -50 °C, about 1 hour after adding, the temperature rising to -30 °C reaction 1 hour, then cooling down to -78 °C; will be 260.4g trimethyl tin chloride (0.8 μM) dissolved with 500 ml of water in tetrahydrofuran, drop into the entry into the above-mentioned mixed solution, keep -78 °C, about 2 hours after the completion of the dropping, natural heating and stirring 8 hours; the ice slowly dripping 500 ml saturated ammonium chloride quenching, filtration, filtrate liquid, collecting the organic phase, the aqueous phase using normal hexane 600 ml × 3 extraction, the combined organic layer, water 600 ml × 3 washing, then the saturated salt water 600 ml × 3 washing, organic uses 90g dried with anhydrous sodium sulfate filter, the filtrate is concentrated under reduced pressure to constant weight, be 249.9g three butyl (α - methoxy ethylene) tin the crude product.The three butyl (α - methoxy ethylene) tin the crude product carries out rectification under vacuum, in the 0.1mmHg vacuum for the temperature of the collection 85 °C -88 °C fraction, shall 211g colorless transparent liquid, yield75.98% ;

References:

CN106046043,2016,A Location in patent:Paragraph 0020; 0021