반응 #566883
ord-0a36fe690e6a48c58cd8470402f0ff46
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용매
반응 조건
후처리
- 1기타Upon reaching 85° C.
- 2온도The reaction was maintained at this temperature for 2.25 h
- 3온도After cooling to RT the mixture
- 4세척then washed with a saturated solution of NH4Cl(aq) (40 ml)
- 5기타The organic layer was separated
- 6건조dried over MgSO4
- 7여과filtered
- 8농축concentrated under reduced pressure
- 9기타The residue was purified by flash chromatography on silica gel (3:1/2:1/1:1, EtOAc:acetone)
실험 절차
To a stirred suspension of 2-bromothiazole-4-carboxylic acid (5.13 g, 2 mmol) in anhydrous CH3CN (40 ml) at RT, under N2, TEA (3.80 ml, 27 mmol) and (PhO)2PON3 (5.90 ml, 27 mmol) were added. The resulting solution was heated to 85° C. Upon reaching 85° C., a solution of 6-(piperidylmethyl)-2-pyridylamine (4.74 g, 25 mmol) in anhydrous CH3CN (60 ml) was added. The reaction was maintained at this temperature for 2.25 h. After cooling to RT the mixture was diluted with CH2Cl2 (50 ml) then washed with a saturated solution of NH4Cl(aq) (40 ml). The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (3:1/2:1/1:1, EtOAc:acetone) to yield the title compound as a pale yellow solid. MS m/z: 396 (M+H), 398 (M+3). Calc'd for C15H18BrN50S: 395.04.