N-bromobutanimide → 2-Bromo-3-methoxycyclopent-2-enone

温度

0 °C

To a stirred solution of 3-methoxy-cyclopent-2-enone (14.95 g, 0.133 mmol) in 1,2-dichloroethane (300 ml) at 0° C. in an amber flask is added portionwise over one hour N-bromosuccinimide (24.92 g, 140 mmol). The reaction is stirred at 0° C. for a further 90 minutes and then any remaining solid is removed by filtration. The filtrate is evaporated to dryness under reduced pressure, the resultant solid dissolved in warm toluene (600 ml) and washed quickly with water (2×100 ml). The organic phase is evaporated under reduced pressure until a precipitate appears. The residue is cooled overnight in a fridge. The resultant solid is removed by filtration, washed with hexane (50 ml) and air-dried to give 15.2 g of 2-bromo-3-methoxy-cyclopent-2-enone as a white crystalline solid.

1. customany remaining solid is removed by filtration
2. customThe filtrate is evaporated to dryness under reduced pressure
3. dissolutionthe resultant solid dissolved in warm toluene (600 ml)
4. washwashed quickly with water (2×100 ml)
5. customThe organic phase is evaporated under reduced pressure until a precipitate
6. temperatureThe residue is cooled overnight in a fridge
7. customThe resultant solid is removed by filtration
8. washwashed with hexane (50 ml)
9. customair-dried

ORDレコード

ord-aa65c74949fb4bfa9d22794d950c92a8

出典データセット

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08889595B2