Sodium Hydroxide → 2-Nitro-3-thiophenecarboxaldehyde

3-Dichloromethyl-2-nitro-thiophene described in Preparation Example T-1 (1.54 g, 7.26 mmol) was dissolved in formic acid (10 mL), and the solution was refluxed for 24 hours under nitrogen atmosphere. An aqueous solution of 5N sodium hydroxide was added to the reaction solution at 0° C., which was then extracted with ethyl acetate, the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1), and the title compound (472 mg, 3.00 mmol, 41%) was obtained as a light brown solid.

1. temperaturethe solution was refluxed for 24 hours under nitrogen atmosphere
2. extractionwhich was then extracted with ethyl acetate
3. washthe organic layer was washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated in vacuo
6. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1)

ORDレコード

ord-4bba1b20929e4db5ab305b46223054d1

出典データセット

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07932272B2