HRID2197481

反应详情

EQUATION

反应方程式

HRID 2197481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 69 (130.4, 0.26 mmol) in methanol (10 mL) was slowly added sodium methoxide (283.8 mg, 5.25 mmol). The mixture was heated to 70° C. for 3 hours at which time Dowex resin was added to quench any remaining methoxide. The resin was filtered off and the solvent evaporated. The product was stirred in 6N HCl over night (16 hr) after which time the solvent was evaporated to give 70 as a white solid, the crude product was carried through to the next step. LCMS: m/z for C20H28N5O4P++H observed 420.2 at 1.92 minutes of a 3.5 minute run, eluting 5-95% CH3CN in H2O.

WORKUP

后处理

  1. additionwas added
  2. customto quench any remaining methoxide
  3. filtrationThe resin was filtered off
  4. customthe solvent evaporated
  5. customwas evaporated