7h-pyrrolo[2,3-d]pyrimidine derivatives
A technology for drugs and compounds, applied in the field of 7H-pyrrolo[2,3-d]pyrimidine derivatives, can solve the problems of low specificity, low bioavailability, large toxic and side effects, etc., and achieve broad market prospects. Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0042] The preparation of embodiment 1 key intermediate of the present invention
[0043] (1) Preparation of 5-iodo-4-amino-7H-pyrrolo[2,3-d]pyrimidine
[0044]
[0045] Weigh 4-amino-7H-pyrrolo[2,3-d]pyrimidine (0.60g, 4.47mmol) and N-iodosuccinimide (1.51g, 6.71mmol) and dissolve in 100ml acetonitrile, and dissolve at 120 Heating at reflux for 24h. After the reaction was completed, the solvent was evaporated, mixed with dichloromethane and water for extraction, the organic phase was dried over anhydrous sodium sulfate, evaporated under reduced pressure, separated and purified by column chromatography to obtain 0.96 g of a yellow solid (yield 82.51%).
[0046] 1 H NMR(500MHz,DMSO-d6)δ13.78(s,1H),8.17(s,1H),7.09(bs,2H).HR-MS(ESI+): Calc.for[C 6 h 5 IN 4 ]:260.9592[M+H]+,found:260.9638[M+H]+,282.9458[M+Na]+.
[0047] (2) Preparation of 5-iodo-7-n-butyl-7H-pyrrolo[2,3-d]pyrimidine 4-amino
[0048]
[0049] Weigh 5-iodo-4-amino-7H-pyrrolo[2,3-d]pyrimidine (2g, 0.0077mo...
Embodiment 2
[0051] Example 2 Preparation of 4-(4-amino-7-n-butyl-7H-pyrrolo[2,3-d]pyrimidine-5-)phenol (compound 1)
[0052]
[0053] 4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)phenol (660 mg, 3.0 mmol) was added to 5-iodo-7-n-butyl After adding base-7H-pyrrolo[2,3-d]pyrimidine 4-amino (177mg, 0.56mmol) in 1,4-dioxane / water (5:1, 25mL:5mL) solution, continue to add carbonic acid Potassium (41.4mg, 3.0mmol) and PdCl 2 (dppf) (4 mg, 0.05 mmol). It was then heated in an oil bath at 90°C for 24 hours. Water and ethyl acetate were added for extraction, and the organic layer was dried over anhydrous magnesium sulfate and evaporated under reduced pressure to obtain 100 mg of white solid (yield 75%).
[0054] 1 H NMR (600MHz, Chloroform-d) δ8.25(s, 1H), 7.55-7.05(d, J=7.4Hz, 4H), 7.01(s, 1H), 6.99(s, 1H), 5.36(s, 2H), 4.26-4.23(t, J=7.2Hz, 2H), 1.89-1.83(m, 2H), 1.41-1.36(m, 2H), 0.89-0.87(d, 3H).HR-MS(ESI+) : Calc.for[C 16 h 18 N 4 O]: 283.1514[M+H]+; Found 283.1552[M+H]+, 305.13...
Embodiment 3
[0055] Example 3 Preparation of 2-(2-(2-(2-(4-(4-amino-7-n-butyl-7H-pyrrolo[2,3-d]pyrimidine-5-)phenoxy)ethyl Oxy)ethoxy)ethoxy)ethyl 4-methylbenzenesulfonic acid (Compound 2)
[0056]
[0057] Tetraethylene glycol bis(p-toluene hydrochloride) (164mg, 3.46mmol), 4-(4-amino-7-n-butyl-7H-pyrrolo[2,3-d]pyrimidine-5-)phenol (100mg , 3.46mmol), and anhydrous potassium carbonate (100mg, 3.46mol) were heated at reflux in 50mL benzene solution for 4h, after neutralization with 1N HCl, the reaction mixture was extracted with dichloromethane. The solution was then dried under reduced pressure to obtain a solid, which was separated by column chromatography to obtain 160 mg of a brown-yellow syrupy product (yield 76%).
[0058] 1 H NMR (600MHz, Chloroform-d)δ8.29(s,1H),δ7.84-6.97(m,8H,arom-H),6.95(s,1H),5.52(s,2H),4.23-4.21 (t,J=7.2Hz,2H),4.23-3.59(t,J=7.2Hz,16H),δ2.44(s,3H),1.87–1.80(m,2H),1.44–1.35(m,2H ),0.97-0.95(t,J=7.4Hz,3H).HR-MS(ESI+): Calc.for[C 31 h 40 N 4 o 7 S]: 613...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 
![7h-pyrrolo[2,3-d]pyrimidine derivatives](https://images-eureka.patsnap.com/patent_img/2b71c65a-6beb-4f06-8c71-fddbadb03605/HDA0001227699750000011.png)
![7h-pyrrolo[2,3-d]pyrimidine derivatives](https://images-eureka.patsnap.com/patent_img/2b71c65a-6beb-4f06-8c71-fddbadb03605/HDA0001227699750000021.png)
![7h-pyrrolo[2,3-d]pyrimidine derivatives](https://images-eureka.patsnap.com/patent_img/2b71c65a-6beb-4f06-8c71-fddbadb03605/BDA0001227699740000011.png)