Stannous Chloride → HCID 14398233, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 12 (0.3 g, 0.9 mmole) in MeOH (7ml) was added carefully a solution of SnCl2 2 H2O (0.72 g, 3.2 mmoles) in concentrated HCl (1 ml). The mixture was stirred at 80° C. for 21/2 hours and the solvent was evaporated. The residue was dissolved in an ice cooled solution of sodium hydroxyde (20 ml, 10N) and extracted with CHCl2. The combined organic extracts were dried, filtered and evaporated to give TLC pure 13 (1.6 g, 95%) as a yellow oil. CC (silica gel: 30 g; eluent: CH2Cl2) afforded 13 (1.55 g, 93) a TLC pure substance. 1H NMR 60 MHz (CDCl3) δ=3.75 (2H, broad s, exchangeable D20) 3.95 (3H, s) 4.4 (2H, s) 6.6-7.3 (4H, m). Mass spectrum, m/z -238/240 (M+).

Provenance & Evidence