HRID9170
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureto reflux for about 12–24 hours
- temperatureUpon cooling
- filtrationThe white precipitate was collected by filtration
- washwas washed well with water
- customLC/MS 2.12 min, 266 (M+1), 264 (M−1), lab LC retention time 4.7 minutes