Thiazole, 2-chloro-5-(2-chloroethyl)-4-methyl- → Clomethiazole

To a solution of 63 g (0.32 moles) of 2-chloro-4-methyl-5-(2-chloroethyl)-thiazole in 630 cm3 of a 96% ethanol 9 g of a wet palladium on charcoal catalyst (palladium content: 8%) are added. The mixture is hydrogenated at atmospheric pressure. The termination of the reaction is indicated by the cease of the hydrogen consumption. After filtering off the catalyst the solution is evaporated, the residue is dissolved in water and the solution is neutralized with sodium hydrogen carbonate (pH 7). The separated oil is shaken out with chloroform. The residue after the evaporation of the chloroform solution is distilled under reduced pressure. 47 g (91%) of 4-methyl-5-(2-chloroethyl)-thiazole are obtained. Its boiling point is 105° C. at a pressure of 0.93 KPa, nD20 =1.5430. Its active agent content is 98.8%, determined by gas chromatography.

1. customcease of the hydrogen consumption
2. filtrationAfter filtering off the catalyst the solution
3. customis evaporated
4. dissolutionthe residue is dissolved in water
5. customThe residue after the evaporation of the chloroform solution
6. distillationis distilled under reduced pressure

ORDレコード

ord-f6d45db65bb345758d8ffd59b2679094

出典データセット

uspto-grants-1996_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05534644