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2.9 Experimental protocol:
2.9.1 General Procedure for the Preparation of Substituted 2-
Aminopyrimidines
In a 50 mL microwave vial were successively dissolved in EtOH (20 mL) 2chloropyrimidine
(3.43 g, 30 mmol), amine (39 mmol, 1.3 equiv) and triethylamine
(6.2 mL, 45 mmol, 1.5 equiv). The reaction tube was sealed, and irradiated in the
cavity of a Milestone MicroSYNTH microwave reactor at a ceiling temperature of
120 °C at 100 W maximum power for 25 min. After the reaction mixture was cooled
with an air flow for 15 min, it was diluted with water (100 mL), extracted with DCM
(2×150 mL) and dried over Na2SO4. The solvent was evaporated in vacuo, and the
crude mixture was purified by silica gel flash chromatography using 0-5%
MeOH−DCM as the eluent.
13 new substituted 2-aminopyrimidine derivatives were synthesized in similar
manner. (Table-1)
Table-1 Compound synthesized
N
N
N
H R
ENTRY CODE R Yield
1 BS-021 cyclododecane 66
2 BS -024 cyclooctane 60
3 BS -025 cycloheptane 64
4 BS -030 cyclobutane 61
5 BS-029 C6H13 88
6 BS -026 C7H15 87
7 BS -027 C8H17 86
8 BS -033 C9H19 86
9 BS -028 C10H21 87
10 BS -034 C11H23 88
11 BS -035 C12H25 89
12 BS -036 C13H27 88
13 BS -037 C14H19 88