反応 #1350582

反応方程式

HCl

dimethyl sulfate

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

NaOH

→

3-Amino-2-methyl-4-methylsulfanylbenzoic Acid

溶媒

toluene

—

ice

water

ethylene glycol

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   workup.WAITAfter 30 min
3. 3
   ろ過the precipitate was filtered off with suction
4. 4
   洗浄washed with water
5. 5
   その他dried

実験手順

10 g of methyl 2-amino-4-methylbenzothiazole-5-carboxylate (0.045 mol.) were dissolved in a mixture of 120 ml of water, 120 ml of ethylene glycol and 50 g of NaOH, and the mixture was stirred at 130° C. for 20 h. The mixture was then diluted with 50 g of ice, 3 drops of (n-Bu)4N+OH— solution were added and finally, at 20° C., 6.25 ml of dimethyl sulfate (0.05 mol) in 15 ml of toluene were added dropwise. After 30 min, the mixture was acidified with conc. HCl and the precipitate was filtered off with suction, washed with water and dried.

出典