5-METHYL-1H-PYRROLO[2,3-B]PYRIDINE synthesis
- Product Name:5-METHYL-1H-PYRROLO[2,3-B]PYRIDINE
- CAS Number:824-52-2
- Molecular formula:C8H8N2
- Molecular Weight:132.16
500903-95-7
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824-52-2
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Yield:824-52-2 80%
Reaction Conditions:
with sodium hydride in 1-methyl-pyrrolidin-2-one;mineral oil at 100; for 0.166667 h;Cooling with ice;
Steps:
1.3 Step 3
Compound 2 (9.8 g, 48.0 mmol) and N-methylpyrrolidone (50 mL) were added to a three-necked flask;Sodium hydride (60%, 2.8 g, 59 mmol) was added to the ice bath,100 degrees Celsius for 10 minutes. Cool to room temperature,Saturated ammonium chloride solution (50 mL) was added and extracted with ethyl acetate (50 mL x 3); the organic phases were combined, washed with water (100 mL) and saturated brine (100 mL), dried over sodium sulphate and filtered. The filtrate was spin dried to give the crude product, which was recrystallized from ethyl acetate (10 mL) to give white solid, compound 3 (5.1 g, 38.6 mmol, 80%).
References:
Kanghua (Shanghai) Drug Discovery Co., Ltd.;Ma Jingxiang CN107056781, 2017, A Location in patent:Paragraph 0008
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