HRID54029

反应详情

EQUATION

反应方程式

HRID 54029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 20 hrs
  2. temperatureThe reaction mixture was cooled
  3. washwashed with water
  4. customdried
  5. customThe removal of solvent
  6. customafforded the solid which
  7. customwas further purified by crystallization