반응 #1797504

반응 방정식

6-methyl-oct-5-en-2-one

sulphuric acid

methanol

→

6-Methoxy-6-methyl-2-octanone

반응 조건

후처리

1. 1
   추출extracted with tert.-butyl methyl ether
2. 2
   세척The combined organic phases were washed with 20% Na2CO3 (200 ml) and concentrated NaCl solution (3×150 ml)
3. 3
   기타After removal of the solvent
4. 4
   workup.DISTILLATIONthe residue was distilled over a 70 cm Sulzer column
5. 5
   기타to give 840 g
6. 6
   기타recovered

실험 절차

To 2 kg 6-methyl-oct-5-en-2-one in 4 l methanol was added 800 ml concentrated sulphuric acid at 3° C. over a period of 40 minutes. After further stirring for 5 h at room temperature, the solution was poured onto 8 kg of ice water and extracted with tert.-butyl methyl ether. The combined organic phases were washed with 20% Na2CO3 (200 ml) and concentrated NaCl solution (3×150 ml). After removal of the solvent, the residue was distilled over a 70 cm Sulzer column to give 840 g recovered starting material (boiling point: 72°-75° C./10 mm Hg) and 970 g 6-methoxy-6-methyl-2-octanone (bp.: 95°-98° C./10 Torr=13.3 mbar).

출처