Sodium Hydroxide → HCID 178507813, compound

Participants

Reaction Steps

The impure product of stage (a) (0.9 g) was dissolved in dry tetrahydrofuran (THF) and added dropwise to a suspension of lithium aluminium hydride (2.0 g) in THF. The mixture was stirred at room temperature for 1 hour and then 2.0 ml of water was added dropwise with caution. A current of air was passed through the mixture for 1 hour and then 0.7 g of sodium hydroxide in 6 ml of water was added. The mixture was filtered and washed with THF. The filtrate was evaporated to dryness leaving an amorphous orange material which was triturated with SVM whereupon orange crystals formed. These were filtered off, washed well with SVM and dried to yield a first crop of product (200 mg) mp210°-215°. The reaction was repeated to give a further crop of product (300 mg) mp200°-210°. The two crops were combined and chromatographed, eluting with chloroform, to give the title compound (350 mg) mp212°-215°.

Provenance & Evidence