반응 #166297

반응 방정식

compound 41

5-Bromo-N4-cyclohexyl-N4-phenyl-pyrimidine-2,4-diamine

K2CO3

→

compound 42

수율 41.7%

9-Cyclohexyl-9H-pyrimido[4,5-b]indol-2-ylamine

수율 41.7%

용매

DMA

반응 조건

후처리

1. 1
   기타was purged with N2 for 20 minutes
2. 2
   온도The reaction was cooled to room temperature
3. 3
   workup.ADDITIONdiluted with ethyl acetate
4. 4
   세척The organic layer was washed with water and brine
5. 5
   건조dried over sodium sulfate
6. 6
   농축concentrated
7. 7
   기타Purification by flash chromatography (ethyl acetate/hexane)

실험 절차

A mixture of compound 41 (0.35 g, 0.99 mmol), Pd(OAc)2 (33 mg, 0.15 mmol), (cyclohexyl)3PBF4 (110 mg, 0.30 mmol), and K2CO3 (138 mg, 0.10 mmol) in DMA (3 mL) was purged with N2 for 20 minutes and then heated at 160° C. for 3 hours. The reaction was cooled to room temperature and diluted with ethyl acetate. The organic layer was washed with water and brine, dried over sodium sulfate and concentrated. Purification by flash chromatography (ethyl acetate/hexane) gave compound 42 as a yellow solid (110 mg, 41%). LCMS-ESI (POS), M/Z, M+1: Found 267.1, Calculated 267.2.

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