Tert-Butylamine → HCID 15729016、化合物

反応式

Cl[C:2]1[N:7]2[N:8]=[C:9]([CH3:13])[C:10](C#N)=[C:6]2[N:5]=[C:4]([CH3:14])[C:3]=1[CH2:15][CH2:16]Cl.C(=O)([O-])[O-].[K+].[K+].[C:24]([NH2:28])([CH3:27])([CH3:26])[CH3:25]>CN(C)C=O>[C:24]([N:28]1[C:2]2[N:7]3[N:8]=[C:9]([C:13]4[CH:16]=[CH:15][CH:3]=[CH:4][CH:14]=4)[CH:10]=[C:6]3[N:5]=[C:4]([CH3:14])[C:3]=2[CH2:15][CH2:16]1)([CH3:27])([CH3:26])[CH3:25]

参加物

実験手順

A mixture of 16.11 g of Compound (VI) [R2 =H, R3 =H], 38 g of anhydrous potassium carbonate, 5.85 g of tert-butylamine, and 140 ml of dimethylformamide was heated at 50°-60° C. in a water bath for 2 days while stirring. The reaction mixture was cooled and filtered. The filtrate was evaporated under reduced pressure. The residue was dissolved in 150 ml of chloroform. The chloroform layer was washed with water and evaporated under reduced pressure to obtain 15.72 g of an oily substance. The oily substance was purified using silica gel chromatography, followed by recrystallizing in a mixed solvent of benzene-isopropylether-hexane to produce 8-tert-butyl-6,7-dihydro-5-methyl-8H-pyrrolo[3,2-e]pyrazolo[1,5-a]pyrimidine [R1 =C(CH3)3, R2 =H, R3 =H in formula (I)] (Compound 11 of this invention) as light yellow plate crystals having a melting point of 147°-149° C. at a yield of 70.1%.