HRID9170

反应详情

EQUATION

反应方程式

HRID 9170 的结构方程式

PROCEDURE

实验过程

About 60 mg N-(6-cyano-1,3-benzothiazol-2-yl)-N′-ethylurea was charged into about 5 mL of about a 1:1 mixture of about 2N aq KOH and dioxane. The reaction mixture was then brought to reflux for about 12–24 hours. Upon cooling, the reaction mixture was poured into about 25 mL of dilute aqueous acid. The white precipitate was collected by filtration and was washed well with water. 1H NMR 1.09 (t, 3H), 3.19 (m, 2H), 6.79 (br s, 1H), 7.65 (d, 1H), 7.92 (m, 1H), 8.48 (d, 1H), 11.0 (br s, 1H), 12.8 (br s, 1H); LC/MS 2.12 min, 266 (M+1), 264 (M−1), lab LC retention time 4.7 minutes.

WORKUP

后处理

  1. temperatureto reflux for about 12–24 hours
  2. temperatureUpon cooling
  3. filtrationThe white precipitate was collected by filtration
  4. washwas washed well with water
  5. customLC/MS 2.12 min, 266 (M+1), 264 (M−1), lab LC retention time 4.7 minutes