反应详情

7-L-arginylamino-4-methylcoumarin hydrochloric acid salt hemihydrate (754 mg, 2 mM) was dissolved in a mixture of DMF (10 ml) and water (10 ml), and carbobenzoxy-L-phenylalanine N-hydroxysuccinimide ester (1.03 g, 2.6 mM) was added thereto. This mixture was stirred for 15 hours at room temperature and concentrated to yield a solid material. The material was purified by column chromatography (2×15 cm) using silica gel as adsorbent and a ternary mixture of chloroform, methylalcohol and acetic acid in 95:5:3 volume ratio. The main fraction was concentrated to yield solid material, dissolved in acetic acid (30 ml) and lyophilized to give 7-(Nα -carbobenzoxy-L-phenylalanyl-L-arginyl)amino-4-methylcoumarin hydrochloric acid salt [XV] (920 mg).

1. additionwas added
2. concentrationconcentrated
3. customto yield a solid material
4. customThe material was purified by column chromatography (2×15 cm)
5. additiona ternary mixture of chloroform, methylalcohol and acetic acid in 95:5:3 volume ratio
6. concentrationThe main fraction was concentrated
7. customto yield solid material