반응 #84655

반응 방정식

2-chloro-6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazoline

tert-butyl ((1S,2S)-2-aminocyclohexyl)carbamate

Cs2CO3

X-Phos

→

tert-butyl ((1S,2R)-2-((6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)amino)cyclohexyl)carbamate

수율 45.3%

용매

DMA

반응 조건

후처리

1. 1
   기타was degassed with N2 for 5 mins
2. 2
   온도The mixture was cooled to room temperature
3. 3
   여과filtered through celite
4. 4
   세척washed with water
5. 5
   기타The residue was purified by silica gel column chromatography

실험 절차

A mixture of 2-chloro-6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazoline (0.1 g, 0.27 mmol), tert-butyl ((1S,2S)-2-aminocyclohexyl)carbamate (75 mg, 0.35 mmol), Cs2CO3 (176 mg, 0.54 mmol), X-Phos (13 mg, 0.027 mmol) and Pd2dba3 (12.5 mg, 0.013 mmol) in DMA (1.8 mL) was degassed with N2 for 5 mins and heated in a microwave reactor at 125° C. for 30 mins. The mixture was cooled to room temperature, filtered through celite and washed with water followed by saturated brine solution. The residue was purified by silica gel column chromatography to afford tert-butyl ((1S,2R)-2-((6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)amino)cyclohexyl)carbamate (67 mg, 45%). MS (ES+) C27H32Cl2N4O4 requires: 546, found: 547 [M+H]+.

출처