Hydrochloric Acid → (2-Chloro-4-methylphenyl)methanol

温度

0 °C

as follows: To a solution of 2-chloro-4-methylbenzoic acid (2.18 g; 12.8 mmol) in THF (22 mL) was added dropwise a solution of BH3.THF in THF (25.6 ml; 1.00 mol/l; 25.6 mmol), at 0° C. Upon complete addition the resulting mixture was heated under reflux, for 3 hours. Subsequently, the mixture was cooled to 0° C., 1M aqueous HCl (30 mL) was added dropwise, and the mixture was stirred for 10 min. Et2O (100 mL) was added and the layers were separated. The organic layer was washed with 1M aqueous HCl (2×), 5% aqueous NaHCO3 (2×), and brine, dried (Na2SO4), filtered and concentrated in vacuo to afford (2-chloro-4-methyl-phenyl)-methanol (1.80 g), which was used as such.

1. customat 0° C
2. additionUpon complete addition the resulting mixture
3. temperaturewas heated
4. temperatureunder reflux, for 3 hours
5. customthe layers were separated
6. washThe organic layer was washed with 1M aqueous HCl (2×), 5% aqueous NaHCO3 (2×), and brine
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated in vacuo

ORDレコード

ord-50db0fbaaa8e4b968395e9a42dc1411a

出典データセット

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09045441B2