Hydrochloric Acid → (5-Fluoromethylpyridin-2-yl)methanol

温度

0 °C

0.45 g of compound (4) dissolved in ethanol is added dropwise to a solution of hydrochloric acid (4.2N) in ethanol (5.5 ml) cooled to 0° C. at the end of the addition, the temperature of the mixture is returned to room temperature and stirring is continued for 12 hours. The reaction mixture is concentrated under vacuum and the residue obtained is washed with isopropyl ether. The ether phase is removed and the residue is taken up in a CH2Cl2/methanol solution (75/25) and then stirred over Na2CO3 (1.2 g). The mixture is filtered and the filtrate evaporated to give a colorless oil (0.3 g), which is used without further purification in the following step.

1. customis returned to room temperature
2. concentrationThe reaction mixture is concentrated under vacuum
3. customthe residue obtained
4. washis washed with isopropyl ether
5. customThe ether phase is removed
6. stirringstirred over Na2CO3 (1.2 g)
7. filtrationThe mixture is filtered
8. customthe filtrate evaporated

ORDレコード

ord-116ffd2b3f14473db3afb52ce5bafc3b

出典データセット

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07547700B2