反応 #63463

反応方程式

sodium hydride

4-(3,4-Dihydro-3-oxo-1,4[2H]-benzothiazin-7-yl)-3-methyl-4-oxobutyric acid

dimethylformamide

methyl iodide

→

Methyl 4-(3,4-dihydro-4-methyl-3-oxo-1,4[2H]-benzothiazin-7-yl)-3-methyl-4-oxobutyrate

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   洗浄The organic layer was washed with brine
3. 3
   乾燥dried over sodium sulfate
4. 4
   その他evaporated
5. 5
   その他The residue was chromatographed on a silica gel column
6. 6
   洗浄eluted with 5% methanol in methylene chloride
7. 7
   その他The solvent was removed
8. 8
   その他the oil obtained

実験手順

4-(3,4-Dihydro-3-oxo-1,4[2H]-benzothiazin-7-yl)-3-methyl-4-oxobutyric acid (1.7 g) was dissolved in 50 ml of dimethylformamide and 0.23 g of 60% sodium hydride was added. After 30 minutes, 0.7 ml of methyl iodide was added and the mixture stirred at room temperature for three hours, then poured into 100 ml of ice water and extracted with ethyl acetate. The organic layer was washed with brine and dried over sodium sulfate and evaporated. The residue was chromatographed on a silica gel column eluted with 5% methanol in methylene chloride. The solvent was removed and the oil obtained was used in Example 56.

出典