HRID723953

反应详情

EQUATION

反应方程式

HRID 723953 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of anhydrous methanol (213 mL) was added sodium methoxide (1.15 g) and 1-(2-amino-benzothiazol-5-yl)-3-benzoyl-thiourea (Example 17, 3.5 g). The resulting mixture was stirred at room temperature for 3 hours. The mixture was concentrated and the residue was poured into water (300 mL). The mixture was extracted using ethyl acetate (3×200 mL). The combined organic fractions were dried over magnesium sulfate, filtered and concentrated (1.61 g, 67%). 1H-NMR (DMSO d6) δ: 9.64 (s, 1H), 760–7.37 (m, 6H), 6.96 (d, 1H, J=8.3 Hz); MS (ESI) 224.8 (M+1, 100%).

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. additionthe residue was poured into water (300 mL)
  3. extractionThe mixture was extracted
  4. dry with materialThe combined organic fractions were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated (1.61 g, 67%)