反应 #166346

反应方程式

compound 269

tert-Butyl 4-(6-((9-cyclopentyl-7-methoxy-9H-pyrido[3′,2′:4,5]pyrrolo[2,3-d]pyrimidin-2-yl)amino)-3-pyridinyl)-1-piperazinecarboxylate

hydrochloric acid

→

compound 270

收率 108.2%

9-Cyclopentyl-2-((5-(1-piperazinyl)-2-pyridinyl)amino)-9H-pyrido[3′,2′:4,5]-pyrrolo[2,3-d]pyrimidin-7-ol

收率 108.2%

反应条件

后处理

1. 1
   其他A 10 mL reaction tube vessel
2. 2
   其他an additional 30 minutes
3. 3
   其他at 140° C
4. 4
   过滤The resulting solution was filtered through a 0.45 μM
5. 5
   过滤filter
6. 6
   洗涤washed with water
7. 7
   其他The solvent was removed in vacuo

实验过程

A 10 mL reaction tube vessel was charged with compound 269 (56.0 mg, 103 μmol) and concentrated hydrochloric acid (2.00 mL, 103 μmol). The reaction was heated with microwave energy (300 W) at 120° C. for 1 hour, then an additional 30 minutes at 140° C. The resulting solution was filtered through a 0.45 μM filter and washed with water. The solvent was removed in vacuo, and the residue coevaporated with water (10 mL) and then methanol (2×, 10 mL) to give compound 270 as a yellow solid (48 mg). 1H NMR (400 MHz, DMSO-d6) δ ppm 11.63-11.91 (m, 2 H) 9.40 (br. s., 4 H) 9.19 (s, 1 H) 8.50 (d, J=8.61 Hz, 1 H) 8.04 (d, J=2.74 Hz, 1 H) 7.99 (dd, J=9.39, 2.74 Hz, 1 H) 7.51 (d, J=9.39 Hz, 1 H) 6.69-6.78 (m, 1 H) 5.35 (quin, J=8.71 Hz, 1 H) 3.37-3.51 (m, 4 H) 3.20-3.34 (m, 4 H) 2.06-2.18 (m, 2 H) 1.93-2.06 (m, 2 H) 1.66-1.82 (m, 2 H) ppm.

来源