HRID2410681

反应详情

EQUATION

反应方程式

HRID 2410681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 7-methoxy-2-(4-methoxyphenyl)-5H-pyrido[3,2-b]indole -4-carboxylate (150 mg, 0 4 mmol) was dissolved in a mixture of tetrahydrofuran (6 mL) and methanol (2 mL) and an aqueous solution of sodium hydroxide (1.0 N, 1.8 mL, 1.8 mmol) was added. After 1 hr the organic solvents were removed on the rotary evaporator and the pH of the aqueous solution was adjusted to about 3 with 6 N aqueous HCl. The resulting precipitate was collected by filtration, washed with water, and dried under vacuum in the presence of KOH to leave 7-methoxy-2-(4-methoxyphenyl)-5H -pyrido[3,2-b]indole-4-carboxylic acid (138 mg, 67% yield) as an orange solid. MS (ESI) m/z 349.1 (M+H). 1H NMR (DMSO-d6) δ ppm 11.47 (1H, s), 8.18 (1H, d, J=8.55 Hz), 8.16 (1H, s), 8.13 (2H, d, J=8.55 Hz), 7.29 (1H, d, J=1.83 Hz), 7.10 (2H, d, J=8.85 Hz), 6.94 (1H, dd, J=8.55, 1.83 Hz), 3.89 (3H, s), 3.85 (3H, s).

WORKUP

后处理

  1. customAfter 1 hr the organic solvents were removed on the rotary evaporator
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. dry with materialdried under vacuum in the presence of KOH