Hydrochloric Acid → (4-Bromopyridin-2-yl)methanamine

温度

0 °C

A solution of 18.70 g of 4-bromopyridine-2-carbonitrile [62150-45-2] in 200 ml of tetrahydrofuran is admixed under argon dropwise with 500 ml of 1M borane-tetrahydrofuran complex solution. The reaction solution is subsequently left to stand at room temperature for 16 hours. The reaction solution is cooled to 0° C., admixed dropwise with 500 ml of 2M HCl and heated to reflux for 30 minutes. The reaction solution is cooled to room temperature, basified with 2M NaOH, saturated with sodium chloride and extracted with tetrahydrofuran (3×300 ml). The combined organic phases are dried over sodium sulphate and concentrated by evaporation. The title compound is identified on the basis of the Rf value from the residue by means of flash chromatography (SiO2 60F).

1. waitThe reaction solution is subsequently left
2. temperatureheated
3. temperatureto reflux for 30 minutes
4. temperatureThe reaction solution is cooled to room temperature
5. extractionextracted with tetrahydrofuran (3×300 ml)
6. dry with materialThe combined organic phases are dried over sodium sulphate
7. concentrationconcentrated by evaporation

ORDレコード

ord-73f2fdd017814be181a76c1c0b1f9e3b

出典データセット

uspto-grants-2011_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07868036B2