Reaktion #1946561

Reaktionsgleichung

2-di-n-butylamino-4-(3-methoxyphenyl)thiazole

compound 2-12

2-di-n-butylamino-4-(3-methoxyphenyl)thiazole

sodium carbonate

phosphorus oxychloride

→

2-Dibutylamino-4-(3-methoxyphenyl)-5-thiazolecarboxaldehyde

Lösungsmittel

DMF

water

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionThe oily precipitate was extracted with methylene chloride
2. 2
   Waschenthe extract was washed with water
3. 3
   Trocknendried over magnesium sulfate
4. 4
   Einengenconcentrated
5. 5
   Sonstigewas used without further purification

Vorschrift

To a solution of 100.8 g (316.5 mmol) of crude 2-di-n-butylamino-4-(3-methoxyphenyl)thiazole (compound 2-12) and 630 ml of DMF was added, over about 30 mins, a solution of 55.81 g (364 mmol) of phosphorus oxychloride in 188 ml of DMF. The mixture was stirred overnight and poured into a solution of 158.1 g of sodium carbonate in 3.5 l of water. The oily precipitate was extracted with methylene chloride, and the extract was washed with water, dried over magnesium sulfate, and concentrated. The yield of brown oil was 88.77 g and was used without further purification. Anal. Calcd. For C19H26N2O2S: C, 65.9; H, 7.6; N, 8.1; S, 9.3. Found: C, 66.20; H, 7.85; N, 8.60; S, 7.93.

Quelle