Sulfuric acid magnesium salt (1:1) → HCID 22912851, compound

Participants

Reaction Steps

Aqueous titanium trichloride (20%, 375 ml) is added dropwise over 15 min to a mixture of N-(6-chloro-2-nitrophenyl)-2-methylalanine methyl ester (XI, EXAMPLE 15, 15.7 g), sodium acetate (268 g), methanol (339 ml) and water (174 ml) at 20°-25°. After stirring for 3 hr at 20°-25°, addition of 950 ml of aqueous sodium bicarbonate, extraction with ethyl acetate several times, stirring with magnesium sulfate and concentration gives the title compound; mp 153°-156°; IR (mineral oil) 3369, 2954, 2924, 2856, 1680, 1594, 1489, 1470, 1450, 1381, 1368, 1357, 1300 and 764 cm-1 ; NMR (CDCl3) 8.25, 6.98, 6.70, 6.6-6.7, 4.25 and 1.45 δ; MS (FAB) m/z 210 and 195.

Provenance & Evidence