반응 #89615

반응 방정식

HCl

methallyl alcohol

methane sulfonic acid

2,6-Dimethyl-cyclohexanone

trimethyl orthoformate

→

2,6-dimethyl-2-(2-methyl-allyl)-cyclohexanone

용매

HOAc

methanol

반응 조건

후처리

1. 1
   기타Reaction
2. 2
   온도the temperature increased from 14° C. to 20° C
3. 3
   기타the reaction mixture was quenched with NaOCH3 (25%, 25 g)
4. 4
   온도heated to 90° C.
5. 5
   온도The reaction mixture was then cooled to room temperature
6. 6
   온도The resulting mixture was heated to 110° C.
7. 7
   온도The reaction mixture was then cooled
8. 8
   세척washed with saturated sodium carbonate solution (3 L)

실험 절차

2,6-Dimethyl-cyclohexanone (1 kg, 4 mol), trimethyl orthoformate (TMOF, 880 g), and methanol (800 mL) were charged to a 5 L reaction flask. HCl was added quickly. Reaction exothermed and the temperature increased from 14° C. to 20° C. The reaction mixture was heated to 60° C. and aged for 7 hours. When the reaction was about 75% complete, the reaction mixture was quenched with NaOCH3 (25%, 25 g), heated to 90° C., and applied to a Bidwell-Sterling trap. The reaction mixture was then cooled to room temperature followed by sequential addition of methallyl alcohol (1.25 Kg, 8.5 moles), HOAc (50 g), and methane sulfonic acid (MSA, 10 g). The resulting mixture was heated to 110° C., applied to a Bidwell-Sterling trap, and aged for 4 hours until gas chromatograph analysis indicated that the reaction was 95% completed. The reaction mixture was then cooled and washed with saturated sodium carbonate solution (3 L) to provide the crude product 2,6-dimethyl-2-(2-methyl-allyl)-cyclohexanone.

출처