HRID1846540

反应详情

EQUATION

反应方程式

HRID 1846540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.15 g (0.59 mmol) spiro[piperidine-4,4′-pyrido[2,3-d][1,3]oxazin]-2′(1′H)-one hydrochloride, 0.15 g (0.55 mmol) 6-(6-chloro-pyrimidin-4-yloxy)-2,4-dimethyl-1H-benzimidazole and 0.31 mL (1.8 mmol) DIPEA were combined in 1.5 mL DMF and stirred first of all overnight at RT then for 2 h at 50° C. The reaction mixture was purified by preparative HPLC-MS. The product-containing fractions were combined and the acetonitrile was evaporated down. The residue was made alkaline with 4N aqueous sodium hydroxide solution, the precipitate formed was suction filtered, washed with water and dried under HV.

WORKUP

后处理

  1. waitfor 2 h at 50° C
  2. customThe reaction mixture was purified by preparative HPLC-MS
  3. customthe acetonitrile was evaporated down
  4. customthe precipitate formed
  5. filtrationfiltered
  6. washwashed with water
  7. customdried under HV