HRID467334

反应详情

EQUATION

反应方程式

HRID 467334 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl 4-methylthio-3-nitrobenzoate (11.7 g) and sodium hydroxide (4.1 g) in ethanol (234 ml) and water (117 ml) was heated at reflux for 2 hours and was then concentrated in vacuo to about 70 ml. Water (250 ml) was added and the mixture was warmed to give a solution which was acidified with acetic acid (30 ml). The mixture was stirred while cooling and the resulting solid collected and washed with water to yield 4-methylthio-3-nitrobenzoic acid (10.3 g), m.p. 245°-247° C. [Elemental analysis: C,45.2; H,3.22; N,6.48; S,14.1%; calculated: C,45.07; H,3.29; N,6.57; S,15.02%].

WORKUP

后处理

  1. temperatureat reflux for 2 hours
  2. concentrationwas then concentrated in vacuo to about 70 ml
  3. additionWater (250 ml) was added
  4. temperaturethe mixture was warmed
  5. customto give a solution which
  6. temperaturewhile cooling
  7. customthe resulting solid collected
  8. washwashed with water