반응 #1946558

반응 방정식

m-anisoyl chloride

potassium thiocyanate

HCl

dibutylamine

→

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

용매

acetone

—

ice water

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도to reflux
3. 3
   온도maintained
4. 4
   온도at reflux for 20 mins
5. 5
   추출The oily residue was extracted with methylene chloride
6. 6
   건조dried over magnesium sulfate
7. 7
   농축concentrated
8. 8
   기타was used without further purification

실험 절차

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.

출처