1. Four substances from the urine of a hypertensive newborn girl were partially characterized and shown to be 17α-hydroxy-5β-pregnane-1,3,20-trione, 3α,17α-dihydroxy-5β-pregnane-1,20-dione, 3α,17α,20α-trihydroxy-5β-pregnan-1-one and 5β-pregnane-1β,3α,17α,20α-tetrol. 2. The characterization rested mainly on RM analysis of the substances and their derivatives by glycol fission, providing evidence for position and degree of substitution and for steroidal character. Supporting evidence was provided by chemically specific location reactions. 3. Certain problems in the manipulation of these β-disubstituted steroids are discussed.

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