Diisopropylethylamine → HCID 57187888、化合物

To 1.52 g (6.85 mmol) of the compound of Example 547B was added 2.75 g (7.44 mmol) of the ethyl (2S,3R,4S)-2-(4-Methoxyphenyl)-4-(1,3-benzodioxol-5-yl)-pyrrolidine-3-carboxylate (prepared by neutralization of the compound of Example 501G), 10 mL of DMSO, and 2 mL of N,N-diisopropylethylamine. The solution was stirred at ambient temperature for 22 h, then poured into 100 mL of water and extracted with diethyl ether (3×25 mL). The combined ether layers were washed with water (1×25 mL), 4% (v/v) H3PO4 (1×25 mL), saturated aqueous NaHCO3 solution (1×25 mL), and brine (1×25 mL), dried over MgSO4, filtered, and concentrated to an oil. This was purified via silica gel chromatography, eluting with 98:2 diethyl ether: methanol to give 3.0 g (79%) of a colorless oil.

1. extractionextracted with diethyl ether (3×25 mL)
2. washThe combined ether layers were washed with water (1×25 mL), 4% (v/v) H3PO4 (1×25 mL), saturated aqueous NaHCO3 solution (1×25 mL), and brine (1×25 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated to an oil
6. customThis was purified via silica gel chromatography
7. washeluting with 98:2 diethyl ether

ORDレコード

ord-7f48d8118ed9434186089dceda9eea52

出典データセット

uspto-grants-2007_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07208517B1