反应详情

A mixture of 6.7 parts of methyl 2-isothiocyanatobenzoate, 8 parts of [1-(2-amino-1-methylethyl)-4-piperidinyl](4-fluorophenyl)methanone and 108 parts of tetrahydrofuran is stirred overnight at room temperature. The reaction mixture is evaporated. The residue is purified twice by column-chromatography over silica gel using first a mixture of trichloromethane and methanol (90:10 by volume) and then a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized twice from 2-propanol, yielding 1.6 parts (13%) of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]propyl]-2,3-dihydro-2-thioxo-4(1H)-quinazolinone; mp. 160.6° C.

1. customThe reaction mixture is evaporated
2. customThe residue is purified twice by column-chromatography over silica gel using first
3. additiona mixture of trichloromethane and methanol (90:10 by volume)
4. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
5. customThe pure fractions are collected
6. customthe eluent is evaporated
7. customThe residue is crystallized twice from 2-propanol