Methyl iodide → Methyl 2-acetamidoethyldithiocarbamate

To a solution of 20.4 g. (0.20 mol) of N-(2-aminoethyl)acetamide in 200 ml. of 95% ethanol was added 27.9 ml. (0.20 mol) of triethylamine and 12.0 ml. (0.20 mol) of carbon disulfide. The exothermic reaction reached reflux and then cooled to ambient temperature over a 1.5 hour period. Methyl iodide (28.4 g; 0.20 ml.) was added which again produced an exothermic reaction. After 1.75 hours the reaction mixture was evaporated to dryness and the solid residue was dissolved in 200 ml. of water. The aqueous solution was extracted twice with 250 ml. portions of ethyl acetate. The extracts were combined, shaken with sodium thiosulfate, dried (MgSO4) and evaporated to dryness to give methyl 2-acetamidoethyldithiocarbamate.

1. customThe exothermic reaction
2. temperaturereached reflux
3. customagain produced
4. customan exothermic reaction
5. customAfter 1.75 hours the reaction mixture was evaporated to dryness
6. dissolutionthe solid residue was dissolved in 200 ml
7. extractionThe aqueous solution was extracted twice with 250 ml
8. dry with materialdried (MgSO4)
9. customevaporated to dryness

ORDレコード

ord-a2ddc4c0581344d993dfba587661d785

出典データセット

uspto-grants-1979_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04174323