HRID2408337

反应详情

EQUATION

反应方程式

HRID 2408337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 250 mL of methanol under nitrogen, 5.21 g of sodium are added. Once dissolution is total and after returning to RT, 20 g of 5,5-dimethyl-4,5-dihydro-imidazol-2-amine bromide and 31.2 g of ethyl malonate are added. The medium is heated with reflux for 16 h. The reaction medium is dry concentrated, and then taken up in 40 mL of ice water. The expected product is precipitated by adding 1N HCl. The obtained precipitate is filtered, washed with water and then dried in the oven at 50° C. 18.62 g (yield=97%) of 7-hydroxy-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one are obtained as a white solid.

WORKUP

后处理

  1. dissolutionOnce dissolution
  2. customafter returning to RT
  3. temperatureThe medium is heated
  4. temperaturewith reflux for 16 h
  5. customThe reaction medium is dry
  6. concentrationconcentrated
  7. customThe expected product is precipitated
  8. additionby adding 1N HCl
  9. filtrationThe obtained precipitate is filtered
  10. washwashed with water
  11. customdried in the oven at 50° C