Hydrogen Sulfide → 3-amino-N,N-dimethyl-3-thioxopropanamide

Temperatur

55 °C

A reaction mixture was prepared from 22.4 g. of N,N-dimethylcyanoacetamide, 21 ml. of liquid hydrogen sulfide and 1 ml. of triethylamine. The reaction mixture was placed in an autoclave and the autoclave shaken at about 55° C. for about 12 hours. The reaction mixture was taken from the autoclave and the volatile constituents removed by evaporation. Ethanol was added to the residue, thus producing a crystalline solid. The solid was filtered and the filter cake washed with cold ethanol. Twenty-one grams of 3-amino-3-thioxo-N,N-dimethylpropanamide were obtained melting at 111°-114° C. The compound had the following nmr (CDCl3 +DMSOd6):δ3.07 (doublet, 6H); 3.82 (singlet, 2H); 9.1 (very broad, 1H).

1. customA reaction mixture was prepared from 22.4 g
2. customthe volatile constituents removed by evaporation
3. additionEthanol was added to the residue
4. customthus producing a crystalline solid
5. filtrationThe solid was filtered
6. washthe filter cake washed with cold ethanol

ORD-Eintrag

ord-92bbd982283a4134830e172fca60ac6b

Quelldatensatz

uspto-grants-1984_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04468399