Benzyl Bromide → HCID 69334435, compound

To a solution of 3-hydroxy-2-nitroestra-1,3,5(10)-trien-17-one (76b, 1.58 g, 5.0 mmol) in DMF (20 mL) were added potassium carbonate (1.38 g, 10 mmol) and benzyl bromide (0.9 mL, 7.5 mmol) and stirred for 19 h at room temperature. To the reaction mixture was added saturated aqueous NH4Cl at 0° C. and extracted with CHCl3. The combined organic layers were washed with H2O, saturated aqueous NaCl, and then dried (Na2SO4). The desiccant was filtered and the solvent was evaporated at reduced pressure. The residue was washed with Et2O to afford 2.01 g of 79 (99% yield) mp: 234-235° C.

1. extractionextracted with CHCl3
2. washThe combined organic layers were washed with H2O, saturated aqueous NaCl
3. dry with materialdried (Na2SO4)
4. filtrationThe desiccant was filtered
5. customthe solvent was evaporated at reduced pressure
6. washThe residue was washed with Et2O

ORD record

ord-6a13a30ca65b420c87bf8d45ddb81421

Source dataset

uspto-grants-2000_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06046186