反应详情

A solution of 3-pyridylcarbinol (2.4 g., 0.0222 mole) in triethylamine (2.24 g., 0.0222 mole) was added dropwise to a solution of N-methyl-(4-methylthiophenyl)carbamoyl chloride in 150 ml. of benzene. The reaction mixture was heated to reflux temperature for about 1 hr. then allowed to stand over night at room temperature. The reaction mixture was washed with water and the benzene layer separated, dried over magnesium sulfate and concentrated in vacuo to give an oil which solidified. The product was recrystallized from methylcyclohexane to give 2.6 g. of solid melting at 100°-102° C. This was a 40.5% yield of 3-pyridylmethyl N-methyl-N-(4-methylthiophenyl)carbamate.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux temperature for about 1 hr
3. waitto stand over night at room temperature
4. washThe reaction mixture was washed with water
5. customthe benzene layer separated
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated in vacuo
8. customto give an oil which
9. customThe product was recrystallized from methylcyclohexane
10. customto give 2.6 g