2-chloroacetoacetamide synthesis
- Product Name:2-chloroacetoacetamide
- CAS Number:67271-66-3
- Molecular formula:C4H6ClNO2
- Molecular Weight:135.55
Yield:67271-66-3 37%
Reaction Conditions:
with sulfuric acid in hydrogenchloride;water;
Steps:
V.a EXAMPLE V
(a) 2-Chloro-3-oxobutyramide From α-chloro-β-aminocrotononitrile: The nitrile (5 g) was added to a solution of sulfuric acid (5 g) in water (10 ml) and the solution kept for two days. This resulted in partial hydrolysis to α-chloro-α-cyanoacetone which formed a separate layer. This was extracted into ether, the ether evaporated, and the residue taken up in conc. HCl (10 ml) and left overnight. A precipitate of ammonium chloride (900 mg) was filtered out and washed with ether, the filtrate was evaporated to a small volume and ether (50 ml) was added. This mixture was dried with Na2 SO4, filtered, evaporated, the residue taken up in warm CH2 Cl2, dried again and evaporated. The residue solidified on standing, it was triturated with a small volume of CH2 Cl2, filtered and washed with CH2 Cl2 and then dried to give 1.54 g of colorless crystals. By concentrating the filtrate to ca. 2 ml a second crop of 0.63 g was obtained (combined yield=37%).
References:
US4214002,1980,A
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