반응 #1702073
ord-a8b5dcdd27e04124891270579f140223
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반응물
시약
반응 조건
후처리
- 1추출extracted by ethyl acetate
- 2세척The organic layer was washed by water
- 3건조a saturated sodium hydrogen carbonate aq. solution and a saturated saline solution, dried over magnesium sulfate
- 4농축concentrated under reduced pressure
- 5기타The crude product was purified by silica gel chromatography
실험 절차
The synthesis process is as set forth in the chemical reaction formula below. The CAN in the reaction path stands for cerium ammonium nitrate. To 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-methylnaphthalene (b) (202 mg, 1.00 mol) were added acetic acid (8.2 mL) and cerium ammonium nitrate (2.40 g, 4.37 mol) followed by stirring at 100° C. for 1 hour. The reaction solution was poured into ice water and extracted by ethyl acetate. 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 (15/1) as an elution solvent. The yield was 106 mg (49%).