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Chemical Structure| 39969-57-8 Chemical Structure| 39969-57-8

Structure of 39969-57-8

Chemical Structure| 39969-57-8

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Product Details of [ 39969-57-8 ]

CAS No. :39969-57-8
Formula : C10H13BrO
M.W : 229.11
SMILES Code : CCCCOC1=CC=C(Br)C=C1
MDL No. :MFCD00037100

Safety of [ 39969-57-8 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H315-H319-H335
Precautionary Statements:P261-P264-P271-P280-P302+P352-P304+P340-P305+P351+P338-P312-P362-P403+P233-P501

Application In Synthesis of [ 39969-57-8 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 39969-57-8 ]

[ 39969-57-8 ] Synthesis Path-Downstream   1~3

  • 2
  • [ 56309-94-5 ]
  • [ 39969-57-8 ]
  • C24H36O4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
90.9% Under a nitrogen atmosphere, well-dried magnesium (2.77 g, 114.08 mmol) and THF (10 mL) were put in a reaction vessel, and the resulting mixture was heated to 40° C. Thereto, 1-bromo-4-butoxybenzene (25.00 g, 109.12 mmol) dissolved in THF (120 mL) was slowly added dropwise in the temperature range of 30° C. to 45° C., and the resulting mixture was further stirred for 30 minutes. A THF (120 mL) solution of <strong>[56309-94-5]4-(1,4-dioxaspiro[4.5]decane-8-yl)cyclohexanone</strong> (23.64 g, 99.20 mmol) was slowly added dropwise in the temperature range of 30° C. to 50° C., and the resulting mixture was further stirred for 60 minutes. The resulting reaction mixture was cooled down to 25° C., and then poured into a saturated aqueous solution of ammonium chloride. The resulting mixture was subjected to extraction with toluene, and the resulting extract was washed with saturated sodium bicarbonate water and water, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain a residue. The residue was purified by silica gel column chromatography (toluene/ethyl acetate=3/1, volume ratio) to obtain compound (T-1) (35.05 g, yield: 90.9percent).
  • 3
  • [ 4441-30-9 ]
  • [ 39969-57-8 ]
  • [ 637-58-1 ]
YieldReaction ConditionsOperation in experiment
82.61% With sodium hydride; In tetrahydrofuran; at 20.0℃; for 5.0h;Reflux; A 500 ml reaction flask was added with 23.2 g (0.1 mol) of the above intermediate.3-morpholine-1-propanol 17.42g (0.12 mol) and 115 g of tetrahydrofuran, with stirring turned on, slowly add 60% sodium hydride 4.8g (0.12 mol), temperature below 20C, about 1~2 min after addition,The reaction was heated to reflux and monitored by TLC. After about 5 hours, the reaction was completed. The solution was concentrated under reduced pressure. 60 ml of water was added and the pH was adjusted to 1 to 2 with concentrated hydrochloric acid.Ethyl acetate (100 ml) was washed twice. The aqueous layer was adjusted to pH 11-12 with 40% sodium hydroxide, and the mixture was extracted twice with 120 ml of ethyl acetate.Combine the organic layers, dry an appropriate amount of anhydrous sodium sulfate, decolorize with 2g of charcoal, concentrate at 40C without concentration, and dissolve with 80ml of methanol.Concentrated hydrochloric acid to adjust the pH 1~2, vacuum concentration to no more, add acetone 40ml dissolved, stirring crystallization, continue to cool to -10 C, stirring crystallization about 6 ~ 8 hours;The mixture was filtered with suction, washed with cold acetone, and dried at 45-50 C. for 6-8 hours to obtain 27.25 g of a white crystalline solid with a yield of 82.61%, a purity of 99.926%, and a maximum single impurity of 0.046%.
 

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