反应详情

To a solution of 4-bromobenzaldehyde (100 g, 0.54 mol) and glycinamide hydrochloride (54 g, 0.48 mol) methanol/water (1500 ml, 5.5/1) was added sodium hydroxide (21.6 g, 0.54 mol). After stirring for 17 h at room temperature the reaction mixture was cooled to 0° C. Sodium borohydride (38 g, 1.0 mol) was added and the mixture was stirred until a clear solution was obtained. The reaction was quenched by addition of concentrated hydrochloric acid until pH=3. After stirring for 17 h the mixture was neutralized with a saturated aqueous solution of sodium hydrogen carbonate and the product was extracted into dichloromethane. The combined organic phases were washed with water, brine, dried over sodium sulfate and concentrated under reduced pressure to afford 2-(4-bromobenzylamino)acetamide (92 g).

1. temperaturewas cooled to 0° C
2. stirringthe mixture was stirred until a clear solution
3. customwas obtained
4. customThe reaction was quenched by addition of concentrated hydrochloric acid until pH=3
5. stirringAfter stirring for 17 h the mixture
6. extractionthe product was extracted into dichloromethane
7. washThe combined organic phases were washed with water, brine
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated under reduced pressure