反応 #5938

反応方程式

2-aminothiophenol

sodium acetate

methyl α-bromo-4-fluorophenylacetate

→

2-(4-fluorophenyl)-3-oxo-3,4-dihydro-2H-1,4-benzothiazine

収率 87.6%

溶媒

ethanol

反応条件

後処理

1. 1
   workup.DISTILLATIONAfter the solvent is distilled off
2. 2
   workup.ADDITIONwater is added to the residue
3. 3
   その他The resulting precipitate is separated by filtration
4. 4
   洗浄washed
5. 5
   その他dried
6. 6
   その他recrystallized from tetrahydrofuran-n-hexane

実験手順

To a suspension of 2-aminothiophenol (12.6 g) and sodium acetate (23.6 g) in ethanol (150 ml) is added methyl α-bromo-4-fluorophenylacetate (23.6 g), and the mixture is stirred at room temperature overnight. After the solvent is distilled off, water is added to the residue. The resulting precipitate is separated by filtration, washed, dried, and then recrystallized from tetrahydrofuran-n-hexane to give 2-(4-fluorophenyl)-3-oxo-3,4-dihydro-2H-1,4-benzothiazine (21.7 g) as crystals. M.p. 216°-219° C.

出典