反应详情

A dichloromethane (20 mL) solution of 11C methylaminal (7.7 g, 20 mmol) is chilled to −78° C. After 20 minutes, allyltrimethylsilane (6.5 mL, 40 mmol) is added. After 10 more minutes 1 M titanium(IV) chloride (24 mL, 24 mmol) is added slowly by syringe. The reaction is complete after 1 hour. The resulting material is carefully quenched (frothing) with saturated bicarb and extracted with dichlormethane, then washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated. The product is isolated by flash chromatography (SiO2), and it crystallizes upon standing. LCMS characterization ES+393.1 (m+1).

1. waitThe reaction is complete after 1 hour
2. customThe resulting material is carefully quenched (frothing) with saturated bicarb
3. extractionextracted with dichlormethane
4. washwashed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe product is isolated by flash chromatography (SiO2), and it
9. customcrystallizes