Sodium borohydride → HCID 20136112, compound

Participants

Reaction Conditions

Reaction Steps

32.9 g (0.10 mol) of 8-(4-chloro-2-fluoro-5-methoxyphenyl)-7-oxo-9-thioxo-1,8-diazabicyclo[4.3.0]nonane were dissolved in 250 ml of ethanol. 5.7 g (0.15 mol) of sodium borohydride were added in portions at a rate such that the temperature was kept at 30° C. When the addition was complete, the mixture was stirred for a further 30 minutes at 30° C. and poured into 600 ml of ice-water. The precipitate was filtered off under suction, dried and recrystallized from methanol. 24.9 g (75% of theory) of 8-(4-chloro-2-fluoro-5-methoxyphenyl)-7-hydroxy-9-thioxo-1,8-diazabicyclo[4.3.0]nonane were obtained in the form of colorless crystals having the melting point 208°-215° C.

Provenance & Evidence