HRID1968292

反应详情

EQUATION

反应方程式

HRID 1968292 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

(R)-3,3-Dimethyl-2-(6-methyl-3-oxo-1-tosylpyrrolo[4,3,2-de][2,6]naphthyridin-4(1H,3H,5H)-yl)butanoic acid (36 mg, 0.079 mmol)) was dissolved in THF (3 mL), MeOH (3 mL) and aqueous NaOH (1N, 3 mL) in a 50 mL round bottom flask. The reaction mixture was heated at 50° C. for 30 min in an oil bath then cooled to room temperature. The solution was concentrated and purified by preparative HPLC (10-35% AcCN/H2O with 0.035% TFA) to give the title compound (10 mg, 42%). 1H NMR (500 MHz, CD3OD) δ 1.25 (s, 9H), 2.29 (s, 3H), 4.87 (s, 1H), 5.21 (d, J=19.5 Hz, 1H), 5.37 (d, J=19.5 Hz, 1H), 7.87 (s, 1H), 8.23 (s, 1H). [M+H] calc'd for C16H19N3O3, 302; found, 302.

WORKUP

后处理

  1. temperaturethen cooled to room temperature
  2. concentrationThe solution was concentrated
  3. custompurified by preparative HPLC (10-35% AcCN/H2O with 0.035% TFA)