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31st January 2013 @ 16:37

 

 

 

Crude product Resynthesis of MD 6-3 (PT-1-4) (31 mg, 62% purity, 54 umol) was dissolved in neat thionyl chloride (3 ml) and stirred overnight at 60°C under a dry nitrogen atmosphere, when TLC (10% MeOH/CHCl3) indicated consumption of starting material. The thionyl chloride was removed in vacuo and replaced by a pyridine solution of H-Sar-OMe•HCl (5eq in 3 ml, 34 mg). The reaction was stirred at room temperature for a further 3 hours, then diluted with EtOAc (20 mL) and washed with 20 ml portions of 2M HCl, sat. Na2CO3 * 2, more HCl, and brine. The organic phase was dried over MgSO4 and evaporated to give a beige solid (PT-1-7A, 14 mg).

 Risks as in Chlorination of PT-1-4A (PT-1-6)

NMR analysis: PT-1-7a was found to consist of silicone grease. Conclusion: All reaction products were water soluble - time-course and mass spectroscopy studies are required.

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