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Paraformaldehyde (1.72 g, 54.3 mmol) was charged in the reactor followed by 100 mL THF and Benzyl-trimethylsilanylmethyl-amine (5) (10 g, 51.7 mmol). 1,1,3,3-tetramethylguanidine (119 mg, 130 μ, 1.03 mmol) was added to the suspension. The reaction mixture was stirred at RT for 1.5 h during which a clear solution was obtained. This solution was added dropwise over 30 min to a mixture consisting of TFA (301 mg, 203 μ, 2.59 mmol) and methyl acrylate (4.95 g, 56.9 mmol). After completion of the reaction (IPC by GC or HPLC, ca 3-5 h), the reaction mixture was concentrated under reduced pressure. The oily residue was dissolved in 25 mL MTBE and was washed twice washed with 60 mL water (60.0 g, 60 mL), then with 30 mL half saturated NaHC03 aq and 25 mL half saturated NaClaq. The organic phase was dried over MgS04, filtered and concentrated under reduced pressure to give 10.4 g of product (21) (89% yield).
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