HRID548761

反应详情

EQUATION

反应方程式

HRID 548761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1,1-dimethylethyl 3-[({3-[(1-methylethyl)oxy]-5-[(4-methyl-5-oxo-2,3,4,5-tetrahydro-1,4-benzoxazepin-8-yl)oxy]phenyl}carbonyl)amino]-1H-pyrazole-1-carboxylate (42 mg, 0.08 mmol), in methanol (2 mL) was heated at 140° C. in a microwave reactor for 30 minutes. The solution was cooled to RT and pressure, the methanol evaporated in vacuo to a residue which was chromatographed on silica, eluting with ethyl acetate, to give the desired compound (13 mg). 1H NMR δ (CDCl3): 1.3 (d, 6H), 3.15 (s, 3H), 3.5 (t, 2H), 4.3 (t, 2H), 4.5 (m, 1H), 6.5 (s, 1H), 6.7 (m, 2H), 6.75 (s, 1H), 7.1 (d, 1H), 7.25 (d, 1H), 7.45 (d, 1H), 7.8 (d, 1H), 9.4 (s, 1H); m/z 437 (M+H)+

WORKUP

后处理

  1. custompressure, the methanol evaporated in vacuo to a residue which
  2. customwas chromatographed on silica
  3. washeluting with ethyl acetate