تفاعل #166297

معادلة التفاعل

compound 41

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

K2CO3

→

compound 42

المردود 41.7%

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

المردود 41.7%

المذيبات

DMA

ظروف التفاعل

المعالجة

1. 1
   أخرىwas purged with N2 for 20 minutes
2. 2
   درجة الحرارةThe reaction was cooled to room temperature
3. 3
   workup.ADDITIONdiluted with ethyl acetate
4. 4
   غسيلThe organic layer was washed with water and brine
5. 5
   تجفيفdried over sodium sulfate
6. 6
   تركيزconcentrated
7. 7
   أخرىPurification by flash chromatography (ethyl acetate/hexane)

الإجراء التجريبي

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.

المصدر