HCID 49797468, compound → HCID 9820646, compound

Participants

Reaction Steps

A solution of pyridinium narcistatin (3a, 0.05 g) in water (2 ml) was obtained by heating (water bath) at 60° C. The solution was allowed to cool prior to passing through a column prepared from Dowex 50X8-200 cation exchange resin (hydrogen form). A suspension began to form in the column as the phosphoric acid (3b) formed. The column was eluted with water and phosphoric acid 3b eluted as a milky white suspension. The combined fractions containing phosphoric acid 3b were freeze dried to afford the product as a colorless solid, (36 mg, 86%); m.p. 175° C. (dec.); 1H NMR (DMSO-d6, 300 MHz), δ 13.65 (s, 1H), 9.02 (s, 1H), 7.06 (s, 1H), 6.48 (s, 1H), 6.17 (d, Jab=10.2 Hz, 1H), 6.06 (m, 2H), 4.46-4.30 (m, 3H), 4.18 (m, 1H); calc for C14H13NO9P 370.0328; found by HR (APCI) [M+H]+ 370.0361.

Provenance & Evidence