反応 #329356

反応方程式

compound

2′-Amino-6′-({[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methyl}thio)-6-{[(4R)-2,2-dimethyl-1,3-dioxolan-4-yl]methoxy}-3,4′-bipyridine-3′,5′-dicarbonitrile

water

→

2′-Amino-6′-({[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methyl}thio)-6-{[(2S)-2,3-dihydroxypropyl]-oxy}-3,4′-bipyridine-3′,5′-dicarbonitrile

溶媒

acetic acid

反応条件

後処理

1. 1
   その他The solvent is then removed on a rotary evaporator
2. 2
   その他the residue is purified directly by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)
3. 3
   その他the product may be purified further by HPLC chromatography on a chiral phase [column: Daicel Chiralpak AS 10 μm, 250 mm×20 mm; mobile phase: isohexane/ethanol 60:40 (v/v); flow rate: 15 ml/min; temperature: 40° C.; detection: 220 nm]

実験手順

95 mg (0.17 mmol) of the compound from example 32A are dissolved in 4 ml of acetic acid. 2 ml of water are then added. The reaction solution is stirred at RT for 12 h. The solvent is then removed on a rotary evaporator, and the residue is purified directly by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5). If required, the product may be purified further by HPLC chromatography on a chiral phase [column: Daicel Chiralpak AS 10 μm, 250 mm×20 mm; mobile phase: isohexane/ethanol 60:40 (v/v); flow rate: 15 ml/min; temperature: 40° C.; detection: 220 nm].

出典