反応 #82307

反応方程式

1-naphthol

N-methylcarbamothioic acid

sodium

→

1-naphthyl N-methylcarbamate

溶媒

benzene

反応条件

後処理

1. 1
   温度the mixture was refluxed for 20 hrs
2. 2
   温度The reaction mixture was cooled
3. 3
   洗浄washed with water
4. 4
   その他dried
5. 5
   その他The removal of solvent
6. 6
   その他afforded the solid which
7. 7
   その他was further purified by crystallization

実験手順

To a solution of 1-naphthol (1.44 g, 0.01 mole) and S-methyl ester of N-methylcarbamothioic acid (1.575 g, 0.015 mole) in benzene (6 ml) there was added sodium (0.15 g) and the mixture was refluxed for 20 hrs. The reaction mixture was cooled and washed with water and a cold 5% NaOH solution followed by water and brine and then dried. The removal of solvent afforded the solid which was further purified by crystallization to furnish 1-naphthyl N-methylcarbamate of the formula VII, m.p. 140°-141° C., IR: 3305 (N--H), 1715 (--COO--), 1600, 1540, 770 (aromatic): PMR (CdCl3, 90 MHz), 2.86 (3H, d, J=1Hz, NH--CH3, 5.14 (1H, hr. s, N--H) and 7.17 to 8 (7H, m, aromatic).

出典