Hydrochloric Acid → HCID 13732639, compound

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Reaction Steps

6.19 g. of the resultant compound of Example 4 suspended in 15 ml. tetrahydrofuran (THF) was treated with 110 ml. 1M BH3 in THF under nitrogen atmosphere. The solution was refluxed 4 hours, then cooled and a solution of 35 ml. concentrated hydrochloric acid and 35 ml. water was added slowly. The solution was refluxed for 20 minutes and then concentrated in vacuum. The residue was made basic with potassium hydroxide solution and extracted with chloroform. The chloroform extracts were dried (K2CO3) and concentrated. The residue was acidified with HCl in isopropyl alochol and this solution was concentrated. Acetonitrile was added to give the product 5.78 g., m.p. 176°-178° C.

Provenance & Evidence