反応 #1934464

反応方程式

7-Hydroxy-3-methyl-4-phenyl-isothiazolo[4,5-c]pyridine-6-carboxylic acid butyl ester

trimethylacetyl chloride

Et3N

→

title compound

収率 80.1%

7-(2,2-Dimethyl-propionyloxy)-3-methyl-4-phenyl-isothiazolo[4,5-c]pyridine-6-carboxylic acid butyl ester

収率 80.1%

溶媒

CH2Cl2

反応条件

後処理

1. 1
   その他The mixture was then quenched with water
2. 2
   抽出extracted with EtOAc (3×10 mL)
3. 3
   洗浄The combined organic layers were washed with brine and water
4. 4
   乾燥dried over MgSO4
5. 5
   濃縮concentrated in vacuo
6. 6
   その他The residue was purified by flash chromatography on silica gel
7. 7
   洗浄Eluting with 0-20% EtOAc/CH2Cl2

実験手順

A mixture of 7-Hydroxy-3-methyl-4-phenyl-isothiazolo[4,5-c]pyridine-6-carboxylic acid butyl ester (1.15 mmol), trimethylacetyl chloride (1.39 mmol), Et3N (1.74 mmol), and CH2Cl2 (5.7 mL) was stirred at r.t. for 2 h. The mixture was then quenched with water and extracted with EtOAc (3×10 mL). The combined organic layers were washed with brine and water, dried over MgSO4, and concentrated in vacuo. The residue was purified by flash chromatography on silica gel. Eluting with 0-20% EtOAc/CH2Cl2 gave the title compound (392.8 mg) as a colorless oil: MS (m/z) 427.2 (M+1).

出典