Diisopropylethylamine → 2-(3,4-dichloro-phenyl)-2-hydroxy-N-[2-(4-hydroxy-3-methoxy-phenyl)-ethyl]-acetamide

To a mixture of (3,4-dichloro-phenyl)-hydroxy-acetic acid (3 g), 4-(2-amino-ethyl)-2-methoxy-phenol hydrochloride (2.7 g) and ethyl-diisopropyl-amine (7 ml) in dimethylformamide (60 ml) is added benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (6 g) in one portion. The mixture is stirred at room temperature for 3 hours. Then water (400 ml) is added. The mixture is extracted with ethyl acetate (2×400 ml) and washed with brine (2×200 ml). The organic layers are collected, dried with MgSO4 and evaporated. 2-(3,4-dichloro-phenyl)-2-hydroxy-N-[2-(4-hydroxy-3-methoxy-phenyl)-ethyl]-acetamide is obtained which is purified by flash column chromatography on silica gel (ethyl acetate/hexane 2:1); the product is an oil.

1. extractionThe mixture is extracted with ethyl acetate (2×400 ml)
2. washwashed with brine (2×200 ml)
3. customThe organic layers are collected
4. dry with materialdried with MgSO4
5. customevaporated

ORD 기록

ord-fb3b917320a7453fb3a75cd7c64f25c4

출처 데이터셋

uspto-grants-2002_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06469005B1