Lenalidomide Impurity 13 synthesis

6synthesis methods

Product Name:Lenalidomide Impurity 13
CAS Number:764-28-3
Molecular formula:C8H12N4
Molecular Weight:164.21

2-Pyridinemethanol, 6-chloro-4-iodo-5-(2-propen-1-yloxy)-

478148-81-1
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764-28-3
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Furo[2,3-c]pyridine-5-methanol, 7-chloro-2,3-dihydro-3-methyl-

478148-82-2
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Yield:478148-82-2 89%

Reaction Conditions:

with tri-n-butyl-tin hydride in benzene;

Steps:

6.v.i EXAMPLE 7(i)

C50 (5.51 g, 16.9 mmol) is suspended in benzene (30 mL) in a dry flask under N₂. Azo(bis)isobutyryl nitrile (289 mg, 1.8 mmol) is added, the mixture is rapidly heated to reflux, and tributyltin hydride (4.91 mL, 18.2 mmol) in benzene (10 mL) is added. The solution is refluxed for 1.5 h, allowed to cool to rt and concentrated in vacuo. The resulting residue is chromatographed over 125 g slurry-packed silica gel, eluding with a gradient of EtOAc/hexane (20%-60%) to afford (7-chloro-3-methyl-2,3-dihydrofuro[2,3-c]pyridin-5-yl)methanol (C51) as a white solid (89% yield). MS (ESI) for C₉H₁₀ClNO₂+H, m/z: 200.1 (M+H).

References:

US2003/153595,2003,A1

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57-06-7 Synthesis