反应详情

温度

95 °C

A mixture of 10.45 g (38.1 mmol) of [2-(2-fluorophenyl)-2-oxoethyl]phosphonic acid diethyl ester and 14.1 g (190 mmol) N-methylethylenediamine in 100 ml of pyridine was heated at 95° C. for 18 hours. The solvent was evaporated and the residue was partitioned between 200 ml of water and 2×100 ml of dichloromethane. The combined organic portions were dried (magnesium sulphate), filtered and evaporated. The residue was purified by column chromatography eluting with 5% methanol/dichloromethane to give 3.14 g (26%) of (1-methyl-1,2,3,4-tetrahydrobenzo[e][1,4]diazepin-5-ylidenemethyl)phosphonic acid diethyl ester as a light brown oil; MS: m/e 311.0 [M+H]+.

1. customThe solvent was evaporated
2. customthe residue was partitioned between 200 ml of water and 2×100 ml of dichloromethane
3. dry with materialThe combined organic portions were dried (magnesium sulphate)
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by column chromatography
7. washeluting with 5% methanol/dichloromethane