反応 #488493

反応方程式

2-tert-butyl-4-fluorophenol

NEt3

methyl chloroformate

→

2-tert-butyl-4-fluorophenyl methyl carbonate

収率 59.0%

溶媒

dioxane

反応条件

後処理

1. 1
   その他The precipitate was removed via filtration
2. 2
   workup.ADDITIONThe filtrate was then diluted with water
3. 3
   抽出extracted with ether
4. 4
   抽出The ether extract
5. 5
   洗浄was washed with water
6. 6
   乾燥dried over MgSO4
7. 7
   その他After removal of solvent
8. 8
   その他the residue was purified by column chromatography

実験手順

To a solution of 2-tert-butyl-4-fluorophenol (2.63 g, 15.7 mmol) and NEt3 (3.13 mL, 22.5 mmol) in dioxane (45 mL) was added methyl chloroformate (1.27 mL, 16.5 mmol). The mixture was stirred at room temperature for 1 h. The precipitate was removed via filtration. The filtrate was then diluted with water and extracted with ether. The ether extract was washed with water and dried over MgSO4. After removal of solvent, the residue was purified by column chromatography to give 2-tert-butyl-4-fluorophenyl methyl carbonate (2.08 g, 59%). 1H NMR (400 MHz, DMSO-d6) δ 7.24 (dd, J=8.8, 5.4 Hz, 1H), 7.17-7.10 (m, 2H), 3.86 (s, 3H), 1.29 (s, 9H).

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