Sodium Dithionite → HCID 131732763, compound

Methyl (3,5-dichloro-2-nitrophenyl)carbamate (79 mg, 0.3 mmol) prepared in Step 1 was added with THF (1.5 mL, 0.2 M), followed by stirring. In a separate vial, sodium hydrosulfite (603 mg, 2.7 mmol, 9.0 eq) and sodium bicarbonate (227 mg, 2.7 mmol, 9.0 eq) were dissolved in H2O (3 mL, 0.1 M), and the solution thus obtained was added to a solution of methyl (3,5-dichloro-2-nitrophenyl)carbamate. MeOH (0.5 mL) was added to the solution, and the mixture was subjected to a reaction at room temperature for 2 hours. Upon completion of the reaction, THF and MeOH were removed by distillation under reduced pressure, and the residue thus obtained was extracted with ethyl acetate (30 mL x 2), dried over MgSO4, and concentrated under reduced pressure. Subsequently, the residue was purified by silica gel column chromatography (EtOAc/Hex=1:4) to obtain the title compound (30 mg, yield: 43%).

1. customthe solution thus obtained
2. customthe mixture was subjected to a reaction at room temperature for 2 hours
3. customwere removed by distillation under reduced pressure
4. customthe residue thus obtained
5. extractionwas extracted with ethyl acetate (30 mL x 2)
6. dry with materialdried over MgSO4
7. concentrationconcentrated under reduced pressure
8. customSubsequently, the residue was purified by silica gel column chromatography (EtOAc/Hex=1:4)

ORD record

ord-423ef1a30ebc4d31b207328d7a90711a

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09018233B2