反应详情

Dissolve 7-chloro-2,5-dimethyl-3-(4-chloro-2,6-dimethylphenyl)-pyrazolo[1,5-a] pyrimidine in 25 mL CH3CN, then add excess ethylenediamine (5 mL) and heat to 80° C. for 3-6 h under N2 with attached reflux condenser. (TLC; product diamine Rf=0.5, aryl chloride Rf=1.0; [10% (2.0M NH3 in MeOH)/90% CH2Cl2] as eluent). Cool to ambient temperature and evaporate to yellow oil. Partition between CH2Cl2 (50 mL) and 1.0 N NaOH (50 mL), and extract aqueous layer 2×30 mL CH2Cl2. Pool organic layers, dry over Na2SO4, filter and evaporate to yellow-white foam (1.25 g). Use without further purification. LCMS=344.4 (MH+); 342.3 (M−).

1. customevaporate to yellow oil
2. customPartition between CH2Cl2 (50 mL) and 1.0 N NaOH (50 mL)
3. extractionextract aqueous layer 2×30 mL CH2Cl2
4. dry with materialPool organic layers, dry over Na2SO4
5. filtrationfilter
6. customevaporate to yellow-white foam (1.25 g)
7. customUse without further purification