Acetic Acid → HCID 70272651, compound

Participants

Reaction Steps

A solution of diazomethane in diethyl ether (generated from N-methyinitroso urea, 623 mg and 40% aqueous potassium hydroxide, 2 mL) was added dropwise to a solution of Example 4 (11.2 mg, 0.0217 mmol) in tetrahydrofuran (2 mL) until a yellow color persisted. Acetic acid was added until yellow color disappeard and the solvents were removed in vacuo. RP-HPLC (45% to 64%, 30 min) gave the titled product (10.3 mg) as a white iyophile. (45% to 64%, 30 min) Tr =13.07 min. 1H NMR (300 MHz, CDCl3) d 1.0 (2×d, J=7.0 Hz, 6H), 1.90 (m, 1H), 2.07 (m, 1H), 2.20 (m, 1H), 2.41 (m, 1H), 3.40 (d, J=16.6 Hz, 1H), 4.21 (s, 3H), 4.36 (d, J=16.6.0 Hz, 1H), 4.70 (m, 1H), 5.20 (sept, J=6.0 Hz, 1H), 6.57 (d, J=7.0 Hz, 1H), 6.88 (m, 4H), 7.10 (m, 4H), 7.21 (br, 2H), 7.38 (m, 4H), 7.59 (d, J=7.0 Hz, 2H), 8.30 (s, 1H). C31H36N4O6 requires m/z 560.6502; found 560.6541.

Provenance & Evidence