Water → 1,3,4-Thiadiazole-2-carbonitrile, 5-(methylthio)-

350 ml tetrahydrofuran were added dropwise upon stirring and cooling at a temperature between 0° and 5° C. to a solution of 20 ml titanium tetrachloride in 50 ml carbon tetrachloride. There were then added at first in batches 15.3 g of 5-methylthio-1,3,4-thiadiazole-2-carboxamide as obtained in Example 11, and thereafter within a period of 1 hour 50 ml triethylamine which had been taken up in 50 ml tetrahydrofuran. After addition of 50 ml water the reaction mixture was extracted with chloroform. The extract was dried on magnesium sulfate and the solvent was removed in a vacuum. The residue was taken up in acetic acid ethylester and filtrated off from the insoluble residue. The ester phase was then treated with activated carbon and finally concentrated to dryness in a vacuum.

1. customas obtained in Example 11
2. extractionwas extracted with chloroform
3. customThe extract was dried on magnesium sulfate
4. customthe solvent was removed in a vacuum
5. filtrationfiltrated off from the insoluble residue
6. additionThe ester phase was then treated with activated carbon
7. concentrationfinally concentrated to dryness in a vacuum

ORD-Eintrag

ord-7136faf88f4a4341ba4c55251d85c8c8

Quelldatensatz

uspto-grants-1981_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04279907