HRID2187493

反应详情

EQUATION

反应方程式

HRID 2187493 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(R)-N-[5-Methyl-8-(4-methylpiperazin-1-yl)-1,2,3,4-tetrahydro-2-naphthyl]-4-morpholinobenzamide (100 mg, 0.22 mmol) was dissolved in tetrahydrofuran (15 mL) and citric acid (51 mg, 0.27 mmol), dissolved in 10% H2O in tetrahydrofuran (5 mL), was added dropwise. The solid material was filtered and recrystallized from a 20% H2O in ethanol (5 mL). The solid was filtered to give 88 mg (62% yield) of white crystals: mp 160° C. (decom.). Anal. Calcd. for C27H36N4O2×C6H8O7×2H2O: C, 57.9; H, 7.6; N, 9.7. Found: C, 58.1; H, 7.4; N, 9.6.

WORKUP

后处理

  1. additionwas added dropwise
  2. filtrationThe solid material was filtered
  3. customrecrystallized from a 20% H2O in ethanol (5 mL)
  4. filtrationThe solid was filtered