反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a round bottom flask was introduced 6-bromo-2-(tetrahydro-2H-pyran-2-yl)-2H-indazol-4-amine (2.77 g) dissolved in DCM (120 ml) followed by the addition of pyridine (1.135 ml). The reaction mixture was left to stir for a few minutes before the addition of 2-methyl-1,3-thiazole-4-carbonyl chloride (2.267 g). The reaction mixture was left to stir at RT for 1 h. After this time the reaction mixture was extracted between DCM and saturated sodium bicarbonate aq. The extracted organic layer was dried down. The crude was dissolved in DCM and adsorbed onto fluorisil before purification by solid loading on companion using Si Column (40 g) eluting with 40-100% ethyl acetate in cyclohexane. The appropriate fractions were combined and evaporated to dryness to yield the title compound, 2.6 g.
WORKUP
后处理
- waitThe reaction mixture was left
- waitThe reaction mixture was left
- extractionAfter this time the reaction mixture was extracted between DCM and saturated sodium bicarbonate aq. The extracted organic layer
- customwas dried down
- dissolutionThe crude was dissolved in DCM
- customadsorbed onto fluorisil before purification by solid loading on companion
- washeluting with 40-100% ethyl acetate in cyclohexane
- customevaporated to dryness