反応 #1702066
ord-2b8a0550c0384e25b553d30943f03be0
反応方程式
反応条件
後処理
- 1洗浄the organic layer was washed by water
- 2乾燥a saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate
- 3濃縮concentrated under reduced pressure
- 4その他The crude product was purified by silica gel chromatography
実験手順
The synthesis process is as set forth in the chemical reaction formula below. The TiCl4 in the reaction path stands for titanium chloride. To 5,6,7,8-tetrahydro-2-hydroxy-5,5,8,8-tetramethylnaphthalene (409 mg, 2.00 mmol) were added titanium chloride (417 mg, 2.20 mmol) and pivaloyl chloride (361 mg, 2.99 mmol) followed by stirring at 120° C. for 1 hour. The reaction solution was diluted by dichloromethane, and the organic layer was washed by water, a saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate, and concentrated under reduced pressure. The crude product was purified by silica gel chromatography using hexane/ethyl acetate (40/3) as an elution solvent. The yield was 53.6 mg (9.0%).