تفاعل #1702067

ord-3e72399696424f17bb8bf6349d4ac7d9

معادلة التفاعل

CC1(C)CCC(C)(C)c2cc(O)ccc21
5,6,7,8-tetrahydro-2-hydroxy-5,5,8,8-tetramethylnaphthalene
ClCCl
dichloromethane
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
O=C(Cl)c1ccccc1
benzoyl chloride
CC1(C)CCC(C)(C)c2cc(C(=O)c3ccccc3)c(O)cc21
5,6,7,8-tetrahydro-3-hydroxy-5,5,8,8-tetramethyl-2-naphthyl phenyl ketone

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted by ethyl acetate
  2. 2
    غسيلThe organic layer was washed by water
  3. 3
    تجفيفa saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate
  4. 4
    تركيزconcentrated under reduced pressure
  5. 5
    أخرىThe crude product was purified by silica gel chromatography

الإجراء التجريبي

The synthesis process is as set forth in the chemical reaction formula below. To 5,6,7,8-tetrahydro-2-hydroxy-5,5,8,8-tetramethylnaphthalene (204 mg, 1.00 mmol) were added anhydrous dichloromethane (1 mL), aluminum chloride (148 mg, 1.12 mmol), and benzoyl chloride (155 mg, 1.10 mmol) followed by stirring at 60° C. for 1 hour. The reaction solution was poured into cold 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 (20/1) as an elution solvent. The yield was 27.3 mg (9%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08765719B2uspto-grants-2014_07