反応 #1946558

反応方程式

m-anisoyl chloride

potassium thiocyanate

HCl

dibutylamine

→

N,N-Dibutyl-N′-(3-methoxybenzoyl)thiourea

溶媒

acetone

—

ice water

反応条件

後処理

1. 1
   温度The mixture was heated
2. 2
   温度to reflux
3. 3
   温度maintained
4. 4
   温度at reflux for 20 mins
5. 5
   抽出The oily residue was extracted with methylene chloride
6. 6
   乾燥dried over magnesium sulfate
7. 7
   濃縮concentrated
8. 8
   その他was used without further purification

実験手順

To a solution of 38.87 g (0.40 mol) of potassium thiocyanate in 630 ml of acetone was added dropwise over 15 min, 68.24 g (0.40 mol) m-anisoyl chloride. The mixture was heated to reflux and maintained at reflux for 20 mins. To this mixture was added 51.7 g (0.40 mol) of dibutylamine over 10 min. The mixture was stirred overnight. The mixture was added to a mixture of 103 ml of conc. HCl in 840 ml of ice water. The oily residue was extracted with methylene chloride, dried over magnesium sulfate and concentrated. The yield of product was 94.62% and was used without further purification. Anal. Calcd. for C17H26N2O2S: C, 63.3; H, 8.1, N, 8.7; S, 9.9. Found: C, 62.54; H, 8.38; N, 8.66: S, 9.19.

出典