HRID541476

反应详情

EQUATION

反应方程式

HRID 541476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into around-bottom flask, was placed a solution of methyl 2,4-dimethyl-5-(6-methyl-3,4,6,7-tetrahydropyrano[3,4-d]imidazol-2-yl)benzoate (compound 464.7, 100 mg, 0.330 mmol, 1.00 equiv) in methanol (10 mL). A solution of lithium hydroxide (76 mg, 3.17 mmol, 10.0 equiv) in water (10 mL) was added and the resulting solution was stiffed for 4 h at room temperature. The mixture was concentrated in vacuo and then aqueous HCl was added until the pH was 5-6. The mixture was adjusted to pH 5-6 with aqueous HCl and then the resulting mixture was concentrated in vacuo. MeOH (5 mL) was added to the residue and the solids were removed by filtration. The filtrate was concentrated in vacuo to obtain the title compound as a yellow solid (60 mg, 63%).

WORKUP

后处理

  1. customInto around-bottom flask, was placed
  2. concentrationThe mixture was concentrated in vacuo
  3. additionaqueous HCl was added until the pH was 5-6
  4. concentrationthe resulting mixture was concentrated in vacuo
  5. additionMeOH (5 mL) was added to the residue
  6. customthe solids were removed by filtration
  7. concentrationThe filtrate was concentrated in vacuo