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
- 100 °C
PROCEDURE
实验过程
A glass microwave reaction vessel was charged with 5-(3-iodo-1-tosyl-1H-indol-5-yl)-N-(4-methoxybenzyl)-1,3,4-thiadiazol-2-amine (543 mg, 0.881 mmol) and N-cyclopropyl-6-(trimethylstannyl)pyrazin-2-amine (350 mg, 1.175 mmol) in DMF (3 mL) followed by copper(i) iodide (223 mg, 1.175 mmol) and Pd(PPh3)4 (67.9 mg, 0.059 mmol). The reaction was stirred and heated in a Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc., Uppsala, Sweden) at 100° C. for 1 h, then diluted with DCM and washed with H2O. The organic layer was dried, filtered and concentrated. The residue was purified with silica gel chromatography (eluting with 20-60% EtOAc in Hex) to give 5-(3-(6-(cyclopropylamino)pyrazin-2-yl)-1-tosyl-1H-indol-5-yl)-N-(4-methoxybenzyl)-1,3,4-thiadiazol-2-amine (130 mg, 0.208 mmol, 17.74% for two steps). MS (ESI, pos. ion) m/z: 624 (M+1).
WORKUP
后处理
- customA glass microwave reaction vessel
- washwashed with H2O
- customThe organic layer was dried
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified with silica gel chromatography (eluting with 20-60% EtOAc in Hex)