Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 86745834, compound

Participants

Reaction Conditions

Reaction Steps

In 10 ml of 2-butanone was dissolved 95 mg of 20-(5,5-dimethyl-1,3-dioxan-2-yl)-1α-(N,N-dimethylcarbamoyl)oxy-3β-(N-phenylcarbamoyl)oxypregna-5,7-diene, followed by addition of 50 mg of pyridinium p-toluenesulfonate, and the mixture was stirred in an atmosphere of argon gas at a temperature of 50° C. for 10 hours. The reaction mixture was then worked up in the same manner as Example 156 to give 45 mg of 1α-(N,N-dimethylcarbamoyl)oxy-3β-(N-phenylcarbamoyl)oxypregna-5,7-diene-20-carbaldehyde showing the following physical properties. 1H-NMR spectrum (90 MHz) δTMSCDCl 3: 0.66 (s, 3H), 1.02 (s, 3H), 1.15 (d, J=6.2 Hz, 3H), 2.78 & 2.81 (each s, 6H), 4.65-5.15 (2H), 5.36 (m, 1H), 5.70 (m, 1H), 6.80 (hr. s, 1H), 7.1-7.7 (5H), 9.60 (d, J= 3.5 Hz, 1H) IR spectrum (KBr): 1725, 1720, 1695 cm-1

Provenance & Evidence