反应详情

温度

0 °C

The aqueous filtrate from the above nucleophilic displacement with disodium salt of 1-carboxymethyl-5-mercaptotetrazole on 4.4 g. of 7-(2-azidomethylphenylacetamido)-3-acetoxymethyl-3-cephem-4-carboxylic acid in 100 ml. of water (or an aqueous solution of II that was adjusted to pH 7 with sodium bicarbonate) was placed in a hydrogenating bottle along with 4 g. of Raney nickel (washed until neutral with water) and shaken for one-half hour at room temperature and 50 psi of hydrogen (Paar hydrogenator). After the catalyst was filtered off, 50 ml. of ethyl acetate was added. The two-layer solution was cooled to 0° C. and then adjusted to pH 2.4 to 3 with 6N hydrochloric acid. The crude 7-(2-aminomethylphenylacetamido)-3-(1-carboxymethyltetrazol-5-ylthiomethyl-3-cephem-4-carboxylic acid that was suspended in the two layer solution was collected by filtration, washed once with 30 ml. of water and once with 30 ml. of ethyl acetate and was dried in vacuum to constant weight. The yield was 3.3 g. or 63.6% of theoretical (estimated by 1c to be 95% pure). A sample was purified and was found to be identical in every way to an authentic sample.

1. filtrationAfter the catalyst was filtered off
2. additionof ethyl acetate was added
3. filtrationwas collected by filtration
4. washwashed once with 30 ml
5. dry with materialof ethyl acetate and was dried in vacuum to constant weight
6. customA sample was purified