Potassium Hydroxide → HCID 66707209, compound

Participants

Reaction Steps

Stir 2-hydroxymethyl[1,3,4]-thiadiazole (241 mg, 2.1 mmol) in thionylchloride (15 mL) for 1 h and concentrate in vacuo. Treat this residue with the thiolate prepared from 3-tert-butoxycarbonyl-6-dimethylcarbamoylthio-2,3,4,5-tetrahydro-1H-benzo[d]azepine (0.4 g, 1.04 mmol) and potassium hydroxide (1.37 g, 24.5 mmol) in methanol (3.5 mL) according to General Procedure 7 to give 3-tert-butoxycarbonyl-7-chloro-6-([1,3,4]thiadiazol-2-yl-methylthio)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (0.3 g, 70%). Treat an aliquot with trifluoroacetic acid to obtain the mass spectrum. MS (ES+) m/z: 312 (M+H)+.

Provenance & Evidence