反応 #1350585

反応方程式

methyl 2-amino-4-methylbenzothiazole-5-carboxylate

NaNO2

hypophosphoric acid

→

Methyl 4-Methylbenzothiazole-5-carboxylate

溶媒

phosphoric acid

water

反応条件

後処理

1. 1
   その他did not exceed −4° C
2. 2
   抽出extracted exhaustively with ethyl acetate
3. 3
   洗浄The organic phases Age were washed
4. 4
   その他dried
5. 5
   その他the solvent was then removed

実験手順

15 g of methyl 2-amino-4-methylbenzothiazole-5-carboxylate (0.07 mol) were initially charged in 450 ml of phosphoric acid, and the mixture was cooled to −8° C. 27.9 g of NaNO2 (0.4 mol) in 30 ml of water were then added dropwise such that the temperature did not exceed −4° C. The diazonium salt was then added dropwise, at 5-10° C., to 169 ml of hypophosphoric acid, and the mixture was stirred at 20° C. overnight. The reaction solution was then neutralized and extracted exhaustively with ethyl acetate. The organic phases Age were washed and dried and the solvent was then removed.

出典