反应详情

2-Hexanone (96.8 g) was added dropwise over 15 min under nitrogen to a stirred suspension of sodium amide (37.7 g) in dry ether (1 liter) at room temperature. The mixture was stirred for 12 min, a solution of methyl methoxyacetate (50.3 g) in dry ether (150 ml) was added dropwise over 20 min, and the mixture was heated under reflux for 2 h. The mixture was cooled, poured into ice and 2N hydrochloric acid (600 ml) and the aqueous layer extracted with ether (4×300 ml). The organic layers were washed with 8% sodium bicarbonate solution and brine, dried and evaporated to give an orange liquid (102 g). Purification by DFC, eluting with System A (5:95) gave a yellow liquid (36 g).

1. temperaturethe mixture was heated
2. temperatureunder reflux for 2 h
3. temperatureThe mixture was cooled
4. extractionthe aqueous layer extracted with ether (4×300 ml)
5. washThe organic layers were washed with 8% sodium bicarbonate solution and brine
6. customdried
7. customevaporated