HRID624308

反应详情

EQUATION

反应方程式

HRID 624308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of methyl 5-iodo-2-methoxy-4-methylbenzoate (3.0 g, 9.80 mmol) in ethanol (10 ml) in a 50 ml RB flask was added an aqueous solution of NaOH (0.784 g, 19.60 mmol, 1M). The reaction mixture was stirred at room temperature overnight. The solvent was removed under vacuum, the solid filtered and dried to give the titled compound (2.2 g, 74%). LCMS: (ES+) m/z=292 (M+H)+; Column. PUROSPHER@star RP-18 (4×55) mm, 3 μm; Buffer: 20 mM NH4OAc IN WATER; Mphase A: Buffer+MeCN (90+10); Mphase B: Buffer+MeCN (10+90); Flow: 2.5 ml/min Time (min.): 0 2 2.5 3; % B: 0 100 100 0; RT: 1.04 min.

WORKUP

后处理

  1. customThe solvent was removed under vacuum
  2. filtrationthe solid filtered
  3. customdried