Butyl bromide → 4-Butoxy-3-methoxybenzonitrile

温度

37 °C

2-methoxy-4-cyano-phenol (0.25 g, 1.67 mmol) and anhydrous DMF (2.00 mL) were added into a flask, then cooled in a water bath while stirring. Several batches of K2CO3 (0.347 g, 2.50 mmol) were added to the mixture and stirred at 20° C. to react for 1 h. n-butyl bromine (0.23 ml, 2.14 mmol) was added into the mixture, which was stirred at room temperature overnight, then heated at 37° C. to react for 6 h. Poured the solution into a mixture of ice/H2O (25 mL), then stirred for 10 min, a precipitate was formed. Filtered, washed with H2O, and air-dried to yield 0.361 g of white solid product with a recovery rate of 92%.

1. temperaturecooled in a water bath
2. stirringstirred at 20° C.
3. additionwas added into the mixture, which
4. stirringwas stirred at room temperature overnight
5. customto react for 6 h
6. additionPoured the solution
7. stirringstirred for 10 min
8. customa precipitate was formed
9. filtrationFiltered
10. washwashed with H2O
11. customair-dried

ORDレコード

ord-530c5479ce4140b091847314f7dece14

出典データセット

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08349835B2