Acetonitrile → Carbonic Acid 10,13-dimethyl-17-(1-methyl-3-octadecylcarbamoyl-propyl)-hexadecahydro-cyclopenta[a]phenanthren-3-yl ester 2,5-dioxo-pyrrolidin-1-yl Ester

Referring to scheme 22, amide 88 (14.5 g, 23 mmol) was dissolved in anhydrous dichloromethane (150 mL). To the solution were added disuccinimidyl carbonate (8.87 g, 34 mmol), triethylamine (15 mL) and acetonitrile (50 mL). The reaction mixture was stirred at room temperature under argon for 6 h and then evaporated dryness. The residue was dissolved in dichloromethane (300 mL). It was washed with saturated NaHCO3 aqueous solution (3×100 mL). The organic layer was dried over Na2SO4, filtered and evaporated to dryness. Compound 89 (14.3 g, 81%) was obtained as colorless powder after drying in high vacuum, which was directly used for the next step without further purification.

1. customevaporated dryness
2. dissolutionThe residue was dissolved in dichloromethane (300 mL)
3. washIt was washed with saturated NaHCO3 aqueous solution (3×100 mL)
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. customevaporated to dryness

ORDレコード

ord-0d9db3a9b7ef4bfd987b8fb1e52bcd30

出典データセット

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07745608B2