Hydrogen Bromide → HCID 86738927, compound

Participants

Reaction Steps

The product of Example I, above, (175.1 mg, 0.39 mmol) was dissolved at room temperature in 2 mL of 32% hydrobromic acid in acetic acid. After 10 min., 40 mL of 2/1 ether/petroleum ether was added. The precipitated solid was separated and dried overnight at room temperature and 5 Pa to yield a glassy, orange foam which was twice dissolved in 1 mL of absolute ethanol and reprecipitated by addition of 30 mL of ether. After drying overnight at room temperature and 5 Pa, there remained 73 mg (44.5%) of white solid; TLC (SiO2 : 10% methanol in methylene chloride) Rf =0.63; mp=190.1°; NMR (CD3OD) δ(LeuCH3)=1.08 D (6), J=5 Hz, δ(LeuCH2) 1.86 D (2), δ(LeuCH)=4.0 M (1), δ(ArH)=7.7 M (9); IR (KBr) C=O=1700 cm-1.

Provenance & Evidence