反应详情

A zinc salt of methotrexate was prepared as follows. Methotrexate (3.0 g, 0.0066 moles) was dissolved in 600 ml methanol at room temperature with rapid stirring. A solution of zinc acetate (0.6 g, 0.0033 moles) in 2 ml methanol was added dropwise to the methotrexate solution. Immediate precipitation (flocculent) was observed. The mixture was stirred for one hour at room temperature. The mixture was then concentrated in a rotating evaporator (roto-vap) at 40° C. The residue obtained (3.2 g) was dried under high vacuum. (C20H22N8O5)2Zn, MW 974.29; percent zinc: 6.46 (found), 6.71 (theoretical).

1. customImmediate precipitation (flocculent)
2. concentrationThe mixture was then concentrated in a rotating evaporator (roto-vap) at 40° C
3. customThe residue obtained (3.2 g)
4. customwas dried under high vacuum