1,2-Dichloroethane → (RS)-N-(4-cyano-benzyl)-2-(2,6-difluoro-3-hydroxy-phenyl)-2-ethoxy-acetamide

温度

0 °C

To an ice cooled mixture under Ar of (RS)-(2,6-difluoro-3-hydroxy-phenyl)-ethoxy-acetic acid, 4-aminomethyl-benzonitrile hydrochloride (10.6 g) and 1-hydroxybenzotriazole (9.8 g) in DMF (140 ml) was added EDC (13.9 g) and triethylamine (55 ml). The mixture was stirred 2.5 h at 0° C. and 2 d at rt. The solvent was evaporated and H2O (250 ml) was added. The product was extracted with AcOEt (2×200 ml). The organic layers were washed with 5% NaHCO3 aq. sol. (100 ml), brine 100 ml). After drying (Na2SO4) the solvent was evaporated. CC (AcOEt/Hept 2:3) afforded 7.66 g (49%) of (RS)-N-(4-cyano-benzyl)-2-(2,6-difluoro-3-hydroxy-phenyl)-2-ethoxy-acetamide. White solid. MS 364.1 ([M+NH4]+).

1. customThe solvent was evaporated
2. additionH2O (250 ml) was added
3. extractionThe product was extracted with AcOEt (2×200 ml)
4. washThe organic layers were washed with 5% NaHCO3 aq. sol. (100 ml), brine 100 ml)
5. dry with materialAfter drying (Na2SO4) the solvent
6. customwas evaporated

ORDレコード

ord-b6daa188619a46f19b7453fd9c40ce6c

出典データセット

uspto-grants-2006_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07129238B2