反応 #1563935

反応方程式

tert-butyl (3-fluoropyridin-4-yl)carbamate

O-(2,4-dinitrophenyl)hydroxylamine

→

1-amino-4-((tert-butoxycarbonyl)amino)-3-fluoropyridin-1-ium 2,4-dinitrophenolate

溶媒

MeCN

MeCN

反応条件

後処理

1. 1
   その他reaction mass
2. 2
   その他reaction mass
3. 3
   濃縮was concentrated at temperature below 40° C. under reduced pressure
4. 4
   その他to afford Int-11 (50 g) which
5. 5
   その他was used in the next step without further purification

実験手順

A solution of tert-butyl (3-fluoropyridin-4-yl)carbamate (25.0 g, 125 mmol) in MeCN (200 ml), was added O-(2,4-dinitrophenyl)hydroxylamine (26.64 g, 125 mmol) in MeCN (200 ml), drop wise over 30 min at RT, reaction mass was stirred at 40° C. for 12 hrs, reaction mass was concentrated at temperature below 40° C. under reduced pressure to afford Int-11 (50 g) which was used in the next step without further purification.

出典