Sodium sulfate decahydrate → HCID 178420359, compound

Participants

Reaction Steps

10 ml of anhydrous tetrahydrofuran solution containing 594 mg (1.5 mmol) of the compound obtained in Example 76 was added dropwise to 5 ml of anhydrous tetrahydrofuran suspension containing 230 mg (6.0 mmol) of lithium aluminum hydride, and the mixture was heated under reflux for 11 hours. Then, 460 mg (12.0 mmol) of lithium aluminum hydride was added and the mixture was again heated under reflux for 3 days. To the reaction mixture was added sodium sulfate decahydrate, the resulting insoluble matter was removed by filtration. The solvent was evaporated and then the resulting residue was purified by a silica gel column chromatography to give 104 mg of the title compound in its free form. By subjecting a 74 mg portion of this compound to salt formation using 33 mg of fumaric acid and recrystallizing it from methanol, 63 mg of the title compound was obtained.

Provenance & Evidence