Diethyl Carbonate → 1-Bromoethyl ethyl carbonate

585 g Diethylcarbonate (4.92 mole) was heated by an external 1500 w iodine quartz lamp. The mixture was allowed to reflux (temperature 125°) by the heat evolved from the lamp. 318.2 g (2.0 mole) of bromine is added slowly during 3 hours through a dip-pipe at such a rate that the solution colour was yellow to light orange. The temperature dropped to ca. 120° at the beginning of the addition, but rose again slowly. When all the bromine was consumed the temperature was 137°. The reaction mixture was cooled and treated as described in Example 2. Fractional distillation afforded 1-bromoethyl ethyl carbonate in a 68.5% yield. The earlier fraction contained about 6.5% more of 1-bromoethyl ethyl carbonate.

1. temperatureto reflux (temperature 125°) by the heat
2. additionThe temperature dropped to ca. 120° at the beginning of the addition
3. customWhen all the bromine was consumed the temperature
4. customwas 137°
5. temperatureThe reaction mixture was cooled
6. additiontreated
7. distillationFractional distillation

ORDレコード

ord-6b42669822d24a26898cdf30aa43b07e

出典データセット

uspto-grants-1989_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04889929