反応 #7703

反応方程式

sodium iodide

2,4-dichloro-5,6,7,8-tetrahydroquinazoline

3-amino-5-cyclopropylpyrazole

triethylamine

→

(2-chloro-5,6,7,8-tetrahydroquinazolin-4-yl)-(5-cyclopropyl-2H-pyrazol-3-yl)-amine

溶媒

DMF

反応条件

後処理

1. 1
   その他The reaction mixture is partitioned between ethyl acetate and aqueous saturated NaHCO3
2. 2
   洗浄The organic layer is washed with brine
3. 3
   その他evaporated in vacuo
4. 4
   その他The residue is purified by flash chromatography (SiO2, hexane/AcOEt gradient)

実験手順

To a solution of 2,4-dichloro-5,6,7,8-tetrahydroquinazoline (500 mg, 2.46 mmol) and 3-amino-5-cyclopropylpyrazole (303 mg, 2.46 mmol) in DMF (10 mL) is added triethylamine (0.357 mL, 2.56 mmol) followed by sodium iodide (368 mg, 2.46 mmol) and the reaction mixture is heated at 90° C. for 20 h. The reaction mixture is partitioned between ethyl acetate and aqueous saturated NaHCO3. The organic layer is washed with brine and evaporated in vacuo. The residue is purified by flash chromatography (SiO2, hexane/AcOEt gradient) to give (2-chloro-5,6,7,8-tetrahydroquinazolin-4-yl)-(5-cyclopropyl-2H-pyrazol-3-yl)-amine.

出典