反応 #77852

反応方程式

3-{5-[3-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl-prop-1-ynyl]pyridin-2-yl}prop-2-ynyl)-1H-isoindole-1,3(2H)-dione

2-(3-{5-[3-(1,3-Dioxo-1,3-dihydro-2H-isoindol-2-yl)prop-1-ynyl]pyridin-2-yl}prop-2-ynyl)-1H-isoindole-1,3(2H)-dione

acetic acid

hydrogen

→

11-1

収率 63.8%

2-(3-{5-[3-(1,3-Dioxo-1,3-dihydro-2H-isoindol-2-yl)propyl]pyridin-2-yl}propyl)-1H-isoindole-1,3(2H)-dione

収率 63.8%

溶媒

DMF

反応条件

後処理

1. 1
   その他The catalyst was removed by filtration through Solka-floc
2. 2
   洗浄washed with ethanol
3. 3
   洗浄The filtrate and wash
4. 4
   濃縮concentrated under reduced pressure

実験手順

A mixture of 2-(3-{5-[3-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl-prop-1-ynyl]pyridin-2-yl}prop-2-ynyl)-1H-isoindole-1,3(2H)-dione (5-1) (200 mg), 10% Pd/C (50 wt %; 60 mg), and acetic acid (1 mL) in DMF (1 mL) was stirred at ambient temperature under 1 atmospheric pressure of hydrogen for 2 days. The catalyst was removed by filtration through Solka-floc and washed with ethanol. The filtrate and wash were combined and concentrated under reduced pressure to give 11-1 (130 mg) as colorless crystals.

出典