Boron trifluoride etherate → 3-(2-Bromoethyl)-2-[(2-bromoethyl)amino]-1,3,2lambda~5~-oxazaphosphinan-2-one

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Reaction Steps

Sodium borohydride (1.5 g) was added to the solution of 6.6 g (18.1 mM) of (+)-3-bromoacetyl-2[(2-bromoethyl)-amino]-2-oxo-1,3,2-oxazaphosphorinane {[α]D25 =+32.7° MeOH} in 45 mL of tetrahydrofuran at ambient temperature and then was added a solution of 5.2 mL of boron trifluoride etherate in 15 mL of tetrahydrofuran. The resulting suspension was stirred at room temperature until completed and then 15 mL of water was added. Following the isolation procedure described in Example II 5.7 g (90%) of the colorless crystalline product was obtained, mp. 93°-94.5° C.; 31P-NMR (CHCl3) δ 11.2 ppm(100%), [α]D25 =+37.86 (c 16 MeOH); TLC (CHCl3 -acetone 3:1) Rf 0.2; MS as in example II

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