Ammonia → 2-Amino-3-cyclopropyl-2-methyl-propionitrile

To a round bottom flask equipped with a condenser was added magnesium sulfate (4.33 g, 35.9 mmol), sodium cyanide (3.52 g, 71.9 mmol) and ammonium chloride (1.92 g, 35.9 mmol). The solids were slurried in a 7.0M solution of ammonia in methanol (30.8 ml, 216 mmol) at room temperature. To the resulting suspension was added 1-cyclopropylpropan-2-one (CAN 4160-75-2, 8.3 g, 71.9 mmol) in one portion. The reaction mixture was stirred at room temperature for 4 hours. The solvents were removed under reduced pressure. The resulting slurry of the inorganic salts and product were diluted with tert-butylmethylether and solvent removed at reduced pressure. This process was repeated three times before the resulting suspension was filtered to remove the inorganic salts. The filtrate was then evaporated down to dryness to yield the crude product (7.9 g, 89%) as a yellow oil. MS (ESI, m/z): 125.3 (M+H+).

1. customTo a round bottom flask equipped with a condenser
2. customThe solvents were removed under reduced pressure
3. additionThe resulting slurry of the inorganic salts and product were diluted with tert-butylmethylether and solvent
4. customremoved at reduced pressure
5. filtrationwas filtered
6. customto remove the inorganic salts
7. customThe filtrate was then evaporated down to dryness

ORD-Eintrag

ord-cbce99c91cb54737a1dfdb27616d092c

Quelldatensatz

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09409866B2