Methanol → HCID 21922995, compound

Participants

Reaction Steps

The operation is carried out as in Stage 2 of Example 7 starting from 280 mg of the product obtained in Stage 1 of Example 7, 4 ml of methanol, 250 mg of 7-methoxy-1,3-benzodioxole-5-carboxaldehyde in place of the benzaldehyde, 0.2 ml of acetic acid and 0.4 ml of tetrahydrofuran and the reaction medium is left for 4 hours at ambient temperature. Then 100 mg of NaBH3CN is added and agitation is carried out at ambient temperature for approximately 3 hours. 10 ml AcOEt is added, followed by washing with 2×5 ml H2O, then 5 ml of saturated aqueous solution of NaCl, followed by drying and evaporating the solvent and purification by chromatography on silica eluting with methylene chloride/methanol/ammonium hydroxide in a proportion of 90/10/1. In this way 311 mg of expected product is obtained in the form of beige crystals.

Provenance & Evidence