反应详情

Ethyl (2R, 3S)-3-hydroxy-2-methylbutyrate (8.20 g) and methyl iodate (78.0 g) were dissolved in N,N-dimethylformamide (150 ml). To this solution was added sodium hydride (about 60% in oil, 2.46 g) little by little with ice cooling and the mixture was stirred for 1 hour with ice cooling. The reaction mixture was poured into ethyl acetate (300 ml) and the mixture was stirred for 10 minutes. Insoluble materials were filtered off and the filtrate was washed 3 times with water. The organic layer was dried, concentrated and distilled under reduced pressure (b.p. 80° C./30 mmHg) to obtain ethyl (2R, 3S)-3-methoxy-2-methylbutyrate (6.87 g).

1. stirringthe mixture was stirred for 10 minutes
2. filtrationInsoluble materials were filtered off
3. washthe filtrate was washed 3 times with water
4. customThe organic layer was dried
5. concentrationconcentrated
6. distillationdistilled under reduced pressure (b.p. 80° C./30 mmHg)