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Take <strong>[60211-57-6]3,5-dichlorobenzyl alcohol</strong> (77 mg, 0.44 mmol, 1.1 equivalents),N,N'-carbonyldiimidazole (77 mg, 0.48 mmol, 1.2 eq.)In a 25 mL single-mouth bottle, DMF was dissolved and stirred at room temperature for 2 h.Compound 2-7 (105 mg, 0.4 mmol) was dissolved in DMF.Add triethylamine (64 muL, 0.48 mmol, 1.2 eq.),The reaction solution was added and stirred at room temperature. TLC tracking monitoring.The oil pump spins off most of the solvent and adds EA and saturated sodium bicarbonate solution.Wash with saturated brine, dry over anhydrous sodium sulfate, spin dry,Cross column (PE: EA = 2:1). A white powder of 150 mg was obtained in a yield of 87.7%.
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 50℃; for 1.5h;
General procedure: Example IV.1 4-{6-Methyl-7-oxo-2,6-diazaspiro[3,4]octan-2-yl}benzonitrile 222 mg (1.81 mmol) 4-Fluorobenzonitrile (CAS No. 1194-02-1) and 320 mg (1.81 mmol) 6-methyl-2,6-diazaspiro[3.4]octan-7-one hydrochloride (CAS No. 2097951-61-4) diluted with 1.6 mL DMSO are treated with 790 mg (5.62 mmol) K2CO3 and stirred at 120 C. for 3 h and at RT overnight. The reaction mixture is cooled and diluted with water. The precipitate is filtered, washed with water and dried in vacuo at 50 C. to yield 340 mg of the product. C14H15N3O (M=241.3 g/mol) ESI-MS: 242 [M+H]+
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 50℃; for 1.5h;
General procedure: Example V.1 4-{6-Methyl-7-oxo-2,6-diazaspiro[3.4]octan-2-yl}benzonitrile 222 mg (1.81 mmol) 4-Fluorobenzonitrile (CAS No. 1194-02-1) and 320 mg (1.81 mmol) 6-methyl-2,6-diazaspiro[3.4]octan-7-one hydrochloride (CAS No. 2097951-61-4) diluted with 1.6 mL DMSO are treated with 790 mg (5.62 mmol) K2CO3 and stirred at 120 C. for 3 h and at RT overnight. The reaction mixture is cooled and is diluted with water. The precipitate is filtered, is washed with water and dried in vacuo at 50 C. to yield 340 mg of the product. C14H15N3O (M=241.3 g/mol) ESI-MS: 242 [M+H]+
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