反应详情

Pyridine diamide 7 was prepared according to the general procedure described in Example 8 using 2-(aminomethyl)pyridine (0.013 mol), 2-chloro-N,N-diisopropylacetamide (0.038 mol), diisopropylethylamine (0.038 mol) and dimethoxyethane (25 mL). The product was isolated from both the methylene chloride extraction of the acidic aqueous layer and the heptane extraction of the basic layer in about equal amounts. Mass spectral analysis of the two layers showed the material in the heptane layer to be of greater purity. The residue from the heptane layer was distilled (150° C., 0.05 mm) to afford 2.2 g of product.

1. customThe product was isolated from both
2. extractionthe methylene chloride extraction of the acidic aqueous layer
3. extractionthe heptane extraction of the basic layer in about equal amounts
4. distillationThe residue from the heptane layer was distilled (150° C., 0.05 mm)