反応 #63813

反応方程式

6(1,1-dimethylethyl)-3-hydroxy-2-phenyl-7-azabenzo[b]thiophene

sodium acetate

→

fine white needles

収率 91.6%

3-Acetoxy-6-(1,1-dimethylethyl)-2-phenyl-7-azabenzo[b]thiophene

収率 91.6%

溶媒

acetic anhydride

反応条件

後処理

1. 1
   温度at reflux for 1 hour
2. 2
   濃縮The solution was concentrated
3. 3
   その他the residue was partitioned between ether and water
4. 4
   洗浄The ether layer was washed with sodium bicarbonate solution and brine
5. 5
   その他dried
6. 6
   濃縮concentrated
7. 7
   その他The residue was crystallized from ether-hexane

実験手順

A solution of 1.42 g (5 mmol) of 6(1,1-dimethylethyl)-3-hydroxy-2-phenyl-7-azabenzo[b]thiophene and 1.42 g sodium acetate in 20 mL of acetic anhydride was heated at reflux for 1 hour. The solution was concentrated and the residue was partitioned between ether and water. The ether layer was washed with sodium bicarbonate solution and brine, dried and concentrated. The residue was crystallized from ether-hexane to afford 1.49 g (91%) of fine white needles, m.p. 128°-9° C.

出典