Ethylene Glycol → HCID 20383037, compound

Participants

Reaction Steps

A solution, prepared at 70°, of 2.83 g of sodium in 200 ml of ethylene glycol is treated with 24.8 g of 8-chloro-1-methylsulphonyloxymethyl-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine (c.f. German Offenlegungsschrift 2,201,210, Example 1) and the mixture is stirred for 6 hours at 70°. The reaction mixture is partitioned between ethyl acetate and water. The organic phase is separated off, washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulphate and evaporated. Crystallisation from ethyl acetate gives 8-chloro-1-(2-hydroxyethoxy-methyl)-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine, melting point 162°-164°.

Provenance & Evidence