تفاعل #70504

معادلة التفاعل

heptane

isopropyl amine

4,5-bis(bromomethyl)-3,6-dichloropyridazine

sodium carbonate

→

solid

المردود 58.2%

1,4-dichloro-6-isopropyl-6H-pyrrolo[3,4-d]pyridazine

المردود 58.2%

المذيبات

THF

THF

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction mixture was concentrated
2. 2
   workup.DISSOLUTIONdissolved in DCM
3. 3
   غسيلwashed with water and brine
4. 4
   تجفيفThe organics solution was dried over Na2SO4
5. 5
   تركيزconcentrated
6. 6
   أخرىto afford a crude oil
7. 7
   أخرىThe mixture was purified by flash chromatography on silica gel
8. 8
   غسيلeluting with 10-80% EtOAc

الإجراء التجريبي

To a suspension of 4,5-bis(bromomethyl)-3,6-dichloropyridazine (700 mg, 2.09 mmol) in 66 mL anhydrous THF was added with sodium carbonate (443 mg, 4.18 mmol) and tetrabutylammonium iodide (77.2 mg, 0.21 mmol). The reaction mixture was added with isopropyl amine (0.18 mL, 2.09 mmol) in 10 mL THF dropwisely for 2 h. The reaction mixture was heated at 70° C. for 3 h. The reaction mixture was concentrated, dissolved in DCM and washed with water and brine. The organics solution was dried over Na2SO4 and concentrated to afford a crude oil. The mixture was purified by flash chromatography on silica gel, eluting with 10-80% EtOAc:heptane to afford a off-white solid (280 mg, yield: 47%).

المصدر