Benzyl Bromide → HCID 71675778、化合物

温度

0 °C

Into a 500-mL 3-neck round-bottom flask, was placed a solution of 4-bromo-3-methyl-1H-pyrazole (20.0 g, 124 mmol) in N,N-dimethylformamide (100 mL). The system was purged with nitrogen, then the solution was cooled to 0° C. Sodium hydride (60% dispersion in mineral oil, 10.0 g, 250 mmol) was carefully added portion-wise and then the resulting mixture was stirred for 30 min at room temperature. The mixture was cooled to 0° C., then benzyl bromide (22.1 mL, 186 mmol) was added drop-wise and the resulting mixture was stirred overnight at room temperature. The mixture was carefully quenched by drop-wise addition of water (40 mL), then the mixture was extracted with ethyl acetate (3×200 mL). The combined organic extracts were washed with brine (4×100 mL), dried (Na2SO4), filleted and concentrated under reduced pressure to obtain the title compound as a yellow oil (24.9 g, 80%).

1. customInto a 500-mL 3-neck round-bottom flask, was placed
2. customThe system was purged with nitrogen
3. temperatureThe mixture was cooled to 0° C.
4. stirringthe resulting mixture was stirred overnight at room temperature
5. customThe mixture was carefully quenched by drop-wise addition of water (40 mL)
6. extractionthe mixture was extracted with ethyl acetate (3×200 mL)
7. washThe combined organic extracts were washed with brine (4×100 mL)
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated under reduced pressure

ORDレコード

ord-701165909e91488da129b4b7a0be58b8

出典データセット

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09428502B2