반응 #507290
ord-bda2f543c4394f1b9d0c998cd2678536
반응 방정식
반응 조건
후처리
- 1기타to form a suspension
- 2온도it was cooled to 0° C
- 3기타to reach at room temperature
- 4workup.ADDITIONwas added at ambient temperature in 10-15 minutes
- 5기타the solvent was recovered under vacuum at 40-45° C
- 6workup.ADDITIONToluene (400 ml) and 5% citric acid solution (750 ml) was added to the recovered solid
- 7여과filtered
- 8기타The solid product obtained
- 9세척was washed with water (750 ml) and hexanes (200 ml)
- 10여과filtered
- 11세척The filtered solid was washed with toluene (200 ml)
- 12기타dried
실험 절차
To dichloromethane (400 ml), D-serine (50 g) was added at ambient temperature under nitrogen atmosphere to form a suspension and then hexamethyldisilazane (134.15 ml) was added to the suspension in 10-15 minutes at ambient temperature. Catalytic amount of ammonium chloride (1 gm) was added. The reaction mixture was refluxed at 35-40° C. for 3 hours and then it was cooled to 0° C. To this mixture, a solution of anhydrous methanol (22.83 g) in dichloromethane (50 ml) was added at 0° C. and the mixture was allowed to reach at room temperature. Triethylamine (48.14 g) was slowly added to it at 25-30° C. and then trityl chloride (132.63 g) was added in 3 lots to the mixture at an interval of 10 minutes. The reaction mixture was then stirred for overnight under nitrogen at ambient temperature. After completion of the reaction, methanol (76.12 g) was added at ambient temperature in 10-15 minutes and the solvent was recovered under vacuum at 40-45° C. Toluene (400 ml) and 5% citric acid solution (750 ml) was added to the recovered solid and filtered. The solid product obtained was washed with water (750 ml) and hexanes (200 ml) and then filtered. The filtered solid was washed with toluene (200 ml) and dried to obtain the titled product. Yield=100 gm; Mass: (-EI): 346 (M−1); 242.9 (-Tr).