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9th May 2013 @ 10:38
Mnr: mnr121-130

Starting material from - Nucleophilic Displacement of MNR99 with 1-Methylpiperazine to give MNR125-1

As for - Bromination of MNR100-2 to give MNR101-2

Hazard Assessment

 

Procedure

MNR125-1 (1.18 g, 5.04 mmol) was dissolved in THF (100 mL) and cooled to -78 °C.  To the stirring solution was added n-BuLi (2.5 M in hexanes, 3.02 mL, 7.55 mmol) and the stirring was continued for 30 minutes.  Bromine (0.52 mL, 10.07 mmol) was added dropwise and the reaction mixture was allowed to reach room temperature and was stirred for 2 hours.  Sodium thiosulfate solution (100 mL) was added and the mixture was extracted with EtOAc (3 x 100 mL).  The organic layers were commbined, dried and filteres then concentrated in vacuo to yield the crude as yellow solid (0.666 g, (100% = 1.57 g)

Poor crude recovery

Attached Files
MNR127-1_table.PNG
MNR127_scheme.png