تفاعل #470983

معادلة التفاعل

2,4-dichloro-6-methylpyrimidine

1,3-thiazol-2-amine

4,5-bis(diphenylphosphino)-9,9-dimethylxanthene

K3PO4

→

2-chloro-6-methyl-N-(1,3-thiazol-2-yl)pyrimidin-4-amine

المذيبات

dioxane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was cooled to room temperature
2. 2
   ترشيحThe insoluble material was filtered off
3. 3
   غسيلwashed with EtOAc
4. 4
   workup.ADDITIONThe filtrate was poured into saturated aqueous solution of NaHCO3
5. 5
   استخلاصextracted with EtOAc
6. 6
   غسيلThe extract was washed with brine
7. 7
   تجفيفdried over Na2SO4
8. 8
   تركيزconcentrated
9. 9
   أخرىThe residue was purified with silica gel column chromatography (eluent: CHCl3/MeOH=98/2˜90/10)

الإجراء التجريبي

To the mixture of 2,4-dichloro-6-methylpyrimidine (507.7 mg), 1,3-thiazol-2-amine (345.0 mg), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (289.1 mg) and K3PO4 (936.3 mg) in dioxane (20 ml) was added Pd2(dba)3 CHCl3 (255.9 mg). And the suspension was stirred at 85° C. overnight. The mixture was cooled to room temperature. The insoluble material was filtered off and washed with EtOAc. The filtrate was poured into saturated aqueous solution of NaHCO3 and extracted with EtOAc. The extract was washed with brine, dried over Na2SO4 and concentrated. The residue was purified with silica gel column chromatography (eluent: CHCl3/MeOH=98/2˜90/10) to give 2-chloro-6-methyl-N-(1,3-thiazol-2-yl)pyrimidin-4-amine as an orange solid.

المصدر