Hydrochloric Acid → HCID 13433566, compound

Temperature

0 °C

0.85 g of 2-cyano-2-propanol and solution F were mixed and stirred for 15 minutes at 0° C. To the mixture was added 0.8 ml of chloroacetic chloride and the solution was stirred for 5 minutes at 0° C., additional 2 hours at room temperature and further 1 hour at 70° C. Then, to the reaction mixture was added 1N hydrochloric acid and water, and extracted with ethyl acetate. The organic layer was washed successively with water and aqueous solution of sodium bicarbonate, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was subjected to silica gel column chromatography to give 0.25 g of (1-cyano-1-methylethyl) chloroacetate.

1. stirringthe solution was stirred for 5 minutes at 0° C., additional 2 hours at room temperature and further 1 hour at 70° C
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed successively with water and aqueous solution of sodium bicarbonate
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue obtained

ORD record

ord-ede42d2471de4f93832a2f69a3bbbc91

Source dataset

uspto-grants-2008_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07439266B2