反应详情

To a stirred suspension of Raney nickel (16 g.) in MeOH (13 ml.) at 0° was added a solution of 3-azidomethyl-7-[2-(2-aminothiazol-4-yl)-2-((Z)-methoxyimino)acetamido]ceph-3-em-4-carboxylic acid (2.96 g.) in MeOH/TFA (14 ml., 1.13 ml.). After effervescence ceased the mixture was diluted with MeOH and filtered through paper. The filtrate was evaporated, the residue purified by HPLC using water/HOAc/MeOH 79:1:20 v/v/v as eluant and the product dried over P2O5 to give 3-aminomethyl-7-[2-(2-aminothiazol-4-yl)-2-((Z)-methoxyimino)acetamido]ceph-3-em-4-carboxylic acid trifluorocetate (yield 45%) having the following n.m.r. in solvent A:--3.5-4.2 (m, 4 H); 3.9 (s, 3 H); 5.15 (d, 1 H); 5.85 (d, 1 H); 6.75 (s, 1 H). The corresponding zwitterionic form was produced by passing an aqueous solution through an ion exchange column.

1. filtrationfiltered through paper
2. customThe filtrate was evaporated
3. customthe residue purified by HPLC
4. dry with materialthe product dried over P2O5