Sodium Acetate → HCID 178470180, compound

Temperature

75 °C

A solution of ethyl aminothioxoacetate (7.4 g) in 74 ml of dichloromethane was stirred in a water bath at room temperature and treated dropwise with triethyloxonium tetrafluoroborate in dichloromethane (1.0M, 74 ml). The mixture was stirred for 16 h and then evaporated to dryness to give a yellow oil. Anhydrous sodium acetate (9.10 g), 2-aminoacetophenone hydrochloride (9.54 g), and glacial acetic acid (110 ml) were added to the oil and the mixture was stirred and heated at 75° C. under an atmosphere of nitrogen. After 2 h the reaction mixture was evaporated and the residue was suspended in water (50 ml), slowly basified with potassium carbonate, and then extracted with ethyl acetate. The organic extracts were washed with water and brine, dried over magnesium sulphate and evaporated to dryness. The residue was crystallized from dichloromethane-diethyl ether to give 7.63 of 4-phenyl-1H-imidazole-2-carboxylic acid ethyl ester.

1. customevaporated to dryness
2. customto give a yellow oil
3. stirringthe mixture was stirred
4. customAfter 2 h the reaction mixture was evaporated
5. extractionextracted with ethyl acetate
6. washThe organic extracts were washed with water and brine
7. dry with materialdried over magnesium sulphate
8. customevaporated to dryness
9. customThe residue was crystallized from dichloromethane-diethyl ether

ORD record

ord-1e67ab5ae4dc4eb58779454f12d5ff8a

Source dataset

uspto-grants-1993_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05254575