Methyl iodide → Methyl 4-bromo-3-methoxythiophene-2-carboxylate

Methyl-3-hydroxy-4-bromo-2-thiophenecarboxylate (10.0 g, 42.2 mmol) was dissolved in 250 mL of acetone. Potassium carbonate (30.0 g, 217.4 mmol) was added followed by a solution of iodomethane (14.5 mL, 233.0 mmol). The mixture was heated to reflux and continued for 6 h. After cooled to room temperature, the mixture was filtered, the solid material was rinsed with acetone (˜200 mL). The filtrate and rinsing were concentrated under reduced pressure to a solid, further dried on high vacuum, yielding 13.7 g (100%) of methyl-3-methoxy-4-bromo-2-thiophenecarboxylate (MH+=251.0),

1. temperatureThe mixture was heated
2. temperatureto reflux
3. filtrationthe mixture was filtered
4. washthe solid material was rinsed with acetone (˜200 mL)
5. washThe filtrate and rinsing
6. concentrationwere concentrated under reduced pressure to a solid
7. customfurther dried on high vacuum

ORDレコード

ord-9f6de7ac8dde43f9b1464dc0799a33c6

出典データセット

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07786149B2