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
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
To a solution of 6-amino-3-pyridinecarbonitrile (30 mg, 0.252 mmol) in pyridine (1 mL) at room temperature, was added 4-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}benzenesulfonyl chloride (84 mg, 0.277 mmol). The reaction mixture was stirred at 20° C. for 30 minutes, then left to stand overnight. The solvent was evaporated in vacuo. The sample was purified by passing through an aminopropyl (NH2) solid phase extraction (SPE) cartridge eluting with methanol, followed by a sulphonic acid (SCX) SPE cartridge eluting with methanol then 2M ammonia/methanol. The product-containing fractions were concentrated to give the title compound (23 mg) as an off-white solid. LCMS (2 min, formic) Rt 0.88 min, m/z (ES+) 385 (M+H)
WORKUP
后处理
- waitleft
- waitto stand overnight
- customThe solvent was evaporated in vacuo
- customThe sample was purified
- extractionby passing through an aminopropyl (NH2) solid phase extraction (SPE) cartridge
- washeluting with methanol
- washeluting with methanol
- concentrationThe product-containing fractions were concentrated